Night vision compatible optical filter resistant to high and low temperatures and high in visible light transmittance and preparation method

文档序号：734310 发布日期：2021-04-20 浏览：7次中文

阅读说明：本技术 一种耐高低温且可见光高透过的夜视兼容滤光片及制备方法 (Night vision compatible optical filter resistant to high and low temperatures and high in visible light transmittance and preparation method ) 是由陶益杰张朝阳袁源郑欣周建伟闫佳于 2020-12-29 设计创作，主要内容包括：本发明公开一种耐高低温且可见光高透过的夜视兼容滤光片及制备方法,该夜视兼容滤光片为层状结构,包括近红外吸收层和增透膜层,增透膜层附着在近红外吸收层的外侧；增透膜层的厚度为40～90μm,近红外吸收层的厚度为0.5～1mm；该制备方法包括近红外吸收层制备、增透保护涂料制备和夜视兼容滤光片制备等步骤。本发明提供的夜视兼容滤光片具有优秀的耐高低温性能,且该夜视兼容滤光片对波段为650～900nm范围内光线具有良好截止性能,其平均透过率仅为0.2％,并在400～630nm的可见光区域的透过率达到50％以上。本发明提供的制备方法工艺简单,制备的夜视兼容滤光片兼顾耐高低温环境、近红外吸收和较高的可见光透过率。(The invention discloses a high and low temperature resistant night vision compatible optical filter with high visible light transmission and a preparation method thereof, the night vision compatible optical filter is of a layered structure and comprises a near infrared absorption layer and an anti-reflection film layer, and the anti-reflection film layer is attached to the outer side of the near infrared absorption layer; the thickness of the anti-reflection film layer is 40-90 mu m, and the thickness of the near-infrared absorption layer is 0.5-1 mm; the preparation method comprises the steps of preparing a near-infrared absorption layer, preparing an anti-reflection protective coating, preparing a night vision compatible optical filter and the like. The night vision compatible optical filter provided by the invention has excellent high and low temperature resistance, has good cut-off performance for light rays within a wave band of 650-900 nm, has an average transmittance of only 0.2%, and has a transmittance of more than 50% in a visible light region of 400-630 nm. The preparation method provided by the invention is simple in process, and the prepared night vision compatible optical filter has high and low temperature environment resistance, near infrared absorption and high visible light transmittance.)

1. The night vision compatible optical filter is characterized by being of a layered structure and comprising a near-infrared absorption layer and an anti-reflection film layer, wherein the anti-reflection film layer is attached to one side of the near-infrared absorption layer; the thickness of the anti-reflection film layer is 40-90 mu m, and the thickness of the near-infrared absorption layer is 0.5-1 mm; the near-infrared absorption layer and the antireflection film layer have the same expansion coefficient and different refractive indexes.

2. The night vision compatible filter of claim 1, wherein the near infrared absorbing layer comprises the following components in parts by mass: 0.1-0.5 part by mass of a near-infrared absorbent, 60-80 parts by mass of an organic solvent and 40-50 parts by mass of a transparent main body resin.

3. The night vision compatible filter of claim 2, wherein the near infrared absorber comprises the following components in parts by mass: 5-20 parts by mass of phthalocyanine dye, 5-20 parts by mass of anthraquinone dye, 10-40 parts by mass of methyl phthalocyanine dye, 20-50 parts by mass of thio-diene type nickel complex dye and 10-40 parts by mass of o-phenylenediamine type complex dye.

4. The night vision compatibility filter of claim 2, wherein the organic solvent is chloroform, toluene or acetone.

5. The night vision compatibility filter of claim 2, wherein the transparent host resin is polymethyl methacrylate.

6. The night vision compatible filter of claim 1, wherein the antireflective film layer comprises the following components in parts by mass: 20-60 parts of polymethyl methacrylate, 5-20 parts of dodecyl trimethoxy silane, 10-30 parts of hexafluorobutyl methacrylate, 10-30 parts of ethyl orthosilicate, 1-10 parts of lanthanum stearate, 1-10 parts of stearic acid and 1-20 parts of nano titanium dioxide.

7. A preparation method of a night vision compatible optical filter resistant to high and low temperatures and high in visible light transmission is characterized by comprising the following steps:

s1: weighing a near-infrared absorbent, an organic solvent and a transparent main body resin according to the mass parts of 0.1-0.5, 60-80 and 40-50, uniformly mixing, placing in a glassware, standing for 24h, transferring to a 100 ℃ oven for completely drying for 1h after the organic solvent is completely volatilized, then performing heat treatment at 120 ℃, and performing hot press molding to obtain a near-infrared absorption layer with the thickness of 0.5-1 mm;

s2: weighing polymethyl methacrylate, dodecyl trimethoxy silane, hexafluorobutyl methacrylate, ethyl orthosilicate, lanthanum stearate, stearic acid and nano titanium dioxide according to the mass parts of 20-60, 5-20, 10-30, 1-10 and 1-20, uniformly mixing, adding into a reaction container, heating to 60-100 ℃, stirring for reaction for 2.0-4.0 h, and cooling to obtain an anti-reflection protective coating;

s3: and spraying an anti-reflection protective coating on the optical mirror surface of the near-infrared absorption layer, drying and curing at 100 ℃, and forming an anti-reflection film layer with the thickness of 40-90 mu m on the near-infrared absorption layer to obtain the night vision compatible optical filter.

8. The method according to claim 7, wherein step S1 specifically includes:

s11: weighing phthalocyanine dye, anthraquinone dye, methyl phthalocyanine dye, thio-diene type nickel complex dye and phthalic diamine type complex dye according to the mass parts of 5-20, 10-40, 20-50 and 10-40, and uniformly mixing to obtain a near-infrared absorbent;

s12: weighing a near-infrared absorbent, an organic solvent and a transparent main body resin according to the mass parts of 0.1-0.5, 60-80 and 40-50, and sealing and drying the transparent main body resin at 80 ℃ for 4 hours;

s13: mixing a near-infrared absorbent, an organic solvent and the dried transparent main body resin, dissolving and stirring for 1-2 hours to obtain a liquid material;

s14: placing the liquid material in a glass ware, standing for 24 hours, transferring the liquid material to a 100 ℃ oven after the organic solvent is completely volatilized, and completely drying for 1 hour to obtain a near-infrared absorbing material;

s15: and carrying out heat treatment on the near-infrared absorption material at 120 ℃, and carrying out hot press molding by using a hot press to obtain the near-infrared absorption layer.

9. The method according to claim 8, wherein in step S12, the organic solvent is chloroform, toluene, or acetone; the transparent main body resin is polymethyl methacrylate;

in step S13, the rotation speed of the dissolving and stirring is 200-300 r/min.

10. The method according to claim 7, wherein in step S2, the stirring reaction is performed at a rotation speed of 200 to 300 r/min.

Technical Field

The invention relates to the technical field of night vision compatible materials, in particular to a night vision compatible optical filter resistant to high and low temperatures and high in visible light transmission and a preparation method thereof.

Background

The night vision compatible technology is to eliminate light and radiation which are emitted by an illumination system and interfere the work of a night vision device through a certain technical means, so that the normal work of the night vision device is ensured. The requirement is that the night vision compatible material has good cut-off performance for 660 nm-900 nm red light region and near infrared red light region, and also needs to ensure enough transmittance in 400 nm-630 nm visible light region. Meanwhile, due to the different environments in which night vision devices are used, the material is required to have excellent high and low temperature resistance. Traditional night vision compatible materials such as colored glass materials, plastic-glass laminated composite materials and the like have the defects of complex process, high price, large mass and the like. The existing night vision compatible materials are simple in process and light in material weight, but the materials are easy to deform in high and low temperature environments and do not have good environmental stability; in addition, although some night vision compatible materials have certain high and low temperature resistance, the transmittance of the material in a visible light region of 400-630 nm is low, which is not beneficial to the application of the night vision compatible materials. Therefore, how to prepare the night vision compatible optical filter with high near infrared absorption and high visible light transmission, which has the characteristics of high and low temperature resistance, becomes a difficult point of current research and development.

Disclosure of Invention

The invention provides a night vision compatible optical filter resistant to high and low temperatures and high in visible light transmission and a preparation method thereof, which are used for overcoming the defects that the high and low temperature resistant environment, near infrared absorption, high visible light transmission rate and the like cannot be considered at the same time in the prior art.

In order to achieve the purpose, the invention provides a night vision compatible optical filter which is resistant to high and low temperatures and high in visible light transmission, wherein the night vision compatible optical filter is of a laminated structure and comprises a near infrared absorption layer and an anti-reflection film layer, and the anti-reflection film layer is attached to the outer side of the near infrared absorption layer; the thickness of the anti-reflection film layer is 40-90 mu m, and the thickness of the near-infrared absorption layer is 0.5-1 mm; the near-infrared absorption layer and the antireflection film layer have the same expansion coefficient and different refractive indexes.

In order to achieve the above object, the present invention further provides a method for manufacturing a night vision compatible optical filter with high temperature resistance and high visible light transmittance, comprising the following steps:

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

1. the night vision compatible optical filter with high temperature resistance, low temperature resistance and high visible light transmission is of a laminated structure and comprises a near-infrared absorption layer and an antireflection film layer, wherein the antireflection film layer is attached to one side of the near-infrared absorption layer; the thickness of the antireflection film layer is 40-90 mu m, the thickness of the near-infrared absorption layer is 0.5-1 mm, the expansion coefficients of the near-infrared absorption layer and the antireflection film layer are consistent, and the refractive indexes are different. The night vision compatible optical filter provided by the invention has excellent high temperature resistance through the structural design and the expansion coefficient and the refractive index of each layer, and still keeps excellent performance in a severe environment, and has good cut-off performance for light rays with the wave band of 650-900 nm, the average transmittance of the optical filter is only 0.2%, and the transmittance of the optical filter in a visible light region with the wave band of 400-630 nm is more than 50%.

2. The preparation method of the high-low temperature resistant high-visible light transmission night vision compatible optical filter provided by the invention is simple in process, the prepared night vision compatible optical filter has good cut-off performance in a red light region of 650-930 nm and a near infrared red light region through a special process and a specific proportioning range, and meanwhile, the prepared night vision compatible optical filter has good transmission rate in a visible light region of 400-630 nm and can be used for a long time in a high-low temperature environment.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.

Fig. 1 is a structural diagram of a night vision compatible filter with high temperature resistance and high visible light transmittance provided by the invention;

fig. 2 is a transmission curve of the optical filter before and after the low-temperature hot-pressing experiment of the near-infrared absorption optical filter prepared in comparative example 1;

fig. 3 is a transmission curve of the optical filter before and after the low-temperature hot-pressing experiment of the night vision compatible optical filter prepared in example 1;

fig. 4 is a transmission curve of the optical filter before and after the low-temperature hot-pressing experiment of the night vision compatible optical filter prepared in example 2;

FIG. 5 is a transmission curve of the optical filter before and after the low temperature hot-pressing experiment of the night vision compatible optical filter prepared in example 3;

fig. 6 is a transmission curve of the optical filter before and after the low-temperature hot-pressing experiment of the night vision compatible optical filter prepared in example 4.

Description of the symbols of the drawings: 1: an anti-reflection film layer; 2: a near infrared absorbing layer.

The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

In addition, the technical solutions in the embodiments of the present invention may be combined with each other, but it must be based on the realization of those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination of technical solutions should not be considered to exist, and is not within the protection scope of the present invention.

The drugs/reagents used are all commercially available without specific mention.

The invention provides a high and low temperature resistant night vision compatible optical filter with high visible light transmission, as shown in figure 1, the night vision compatible optical filter is of a layered structure and comprises a near infrared absorption layer 2 and an anti-reflection film layer 1, wherein the anti-reflection film layer 1 is attached to one side of the near infrared absorption layer 2; the thickness of the anti-reflection film layer 1 is 40-90 mu m, and the thickness of the near-infrared absorption layer 2 is 0.5-1 mm; the near-infrared absorption layer 2 and the antireflection film layer 1 have the same expansion coefficient and different refractive indexes, so that high and low temperature resistance and high visible light transmission are achieved.

Preferably, the near-infrared absorption layer comprises the following components in parts by mass: 0.1-0.5 part by mass of a near-infrared absorbent, 60-80 parts by mass of an organic solvent and 40-50 parts by mass of a transparent main body resin.

Preferably, the near-infrared absorbent comprises the following components in parts by mass: 5-20 parts by mass of phthalocyanine dye, 5-20 parts by mass of anthraquinone dye, 10-40 parts by mass of methyl phthalocyanine dye, 20-50 parts by mass of thio-diene type nickel complex dye and 10-40 parts by mass of o-phenylenediamine type complex dye.

Preferably, the organic solvent is chloroform, toluene or acetone, and has good solubility and easy volatilization.

Preferably, the transparent host resin is polymethyl methacrylate.

Preferably, the antireflection film layer comprises the following components in parts by mass: 20-60 parts of polymethyl methacrylate, 5-20 parts of dodecyl trimethoxy silane, 10-30 parts of hexafluorobutyl methacrylate, 10-30 parts of ethyl orthosilicate, 1-10 parts of lanthanum stearate, 1-10 parts of stearic acid and 1-20 parts of nano titanium dioxide.

The main component of the anti-reflection film layer is the same as that of the near-infrared absorption layer, namely resin, and the refractive indexes of the anti-reflection film layer and the near-infrared absorption layer are changed by respectively adding other components such as nano titanium dioxide and lanthanum stearate, so that the anti-reflection film layer and the near-infrared absorption layer have the same expansion coefficient but different refractive indexes, and the purposes of high and low temperature resistance and high visible light transmittance are achieved.

The invention also provides a preparation method of the night vision compatible optical filter with high temperature resistance and high visible light transmission, which comprises the following steps:

Preferably, step S1 specifically includes:

s13: mixing a near-infrared absorbent, an organic solvent and the dried transparent main body resin, dissolving and stirring for 1-2 hours to obtain a liquid material;

s15: and carrying out heat treatment on the near-infrared absorption material at 120 ℃, and carrying out hot press molding by using a hot press to obtain the near-infrared absorption layer.

Preferably, in step S12, the organic solvent is chloroform, toluene or acetone; the transparent main body resin is polymethyl methacrylate;

in step S13, the rotation speed of the dissolving and stirring is 200-300 r/min.

Preferably, in step S2, the rotation speed of the stirring reaction is 200 to 300 r/min.

Comparative example 1

The comparative example provides a method for preparing a near-infrared absorption filter, comprising the following steps:

(1) weighing 10 parts by mass of phthalocyanine dye, 10 parts by mass of anthraquinone dye, 20 parts by mass of methyl phthalocyanine dye, 25 parts by mass of thio-diene type nickel complex dye and 30 parts by mass of o-phenylenediamine type complex dye according to the parts by mass of the near-infrared absorbent, and uniformly mixing;

(2) weighing the near-infrared absorbent, chloroform and polymethyl methacrylate according to the mass parts of 0.2, 60 and 40, and sealing and drying the polymethyl methacrylate at the temperature of 80 ℃ for 4 hours;

(3) mixing, dissolving and stirring a near-infrared absorbent, chloroform and dried polymethyl methacrylate for 1-2 hours, and setting the rotating speed to be 200-300 r/min to obtain a liquid material;

(4) placing the liquid material obtained in the third step in a glass ware, standing for 24 hours, transferring the liquid material to a 100 ℃ oven after the chloroform is completely volatilized, and completely drying for 1 hour to obtain a near-infrared absorbing material;

(5) and carrying out heat treatment on the near-infrared absorption material at 120 ℃, and carrying out hot press molding by adopting a hot press to obtain the smooth and flat near-infrared absorption optical filter with the thickness of 1.0 mm.

The near-infrared absorption filter of the comparative example was evaluated for transmission test using an ultraviolet/visible/near-infrared spectrophotometer, and the test results are listed in table 1:

table 1: average transmittance at normal temperature, hot storage and cold storage of the near-infrared absorption filter of comparative example 1

Evaluation item	Comparative example 1	Storing at 80 deg.C for 200h	Cold storage at 0 deg.C for 24 hr
				Average transmittance of 400-630 nm light	34.74％	35.04％	35.04％
Average light transmittance of 650-930 nm	0.14％	0.15％	0.14％

Example 1

The embodiment provides a night vision compatible optical filter which is resistant to high and low temperatures and high in visible light transmission, wherein the night vision compatible optical filter is of a laminated structure and comprises a near-infrared absorption layer and an antireflection film layer, and the antireflection film layer is attached to one side of the near-infrared absorption layer; the thickness of the anti-reflection film layer is 60 micrometers, and the thickness of the near-infrared absorption layer is 1.0 mm; the near-infrared absorption layer and the antireflection film layer have the same expansion coefficient and different refractive indexes.

The embodiment also provides a method for manufacturing the night vision compatible optical filter with high temperature resistance, low temperature resistance and high visible light transmittance, which includes the following steps:

(1) comparative example 1 to (4);

(5) carrying out heat treatment on the near-infrared absorption material at 120 ℃, and carrying out hot press molding by using a hot press to obtain a smooth and flat near-infrared absorption layer with the thickness of 1.0 mm;

(6) weighing polymethyl methacrylate, dodecyl trimethoxy silane, hexafluorobutyl methacrylate, ethyl orthosilicate, lanthanum stearate, stearic acid and nano titanium dioxide according to parts by mass of 40, 10, 20, 5 and 10, uniformly mixing, adding into a reaction container, heating to 60-100 ℃, stirring for reaction for 2.0-4.0 h, and cooling to obtain an anti-reflection protective coating;

(7) and spraying anti-reflection protective coating on the optical mirror surface of the smooth and flat near-infrared absorption layer, drying and curing at 100 ℃, and forming an anti-reflection film layer with the thickness of 60 mu m on the near-infrared absorption layer to obtain the night vision compatible optical filter.

The night vision compatible filter prepared in this example was evaluated in a transmission test using an ultraviolet/visible/near infrared spectrophotometer, and the test results are listed in table 2:

table 2: the near-infrared absorption filter of example 1 had average transmittances at room temperature, hot storage and cold storage

Evaluation item	Example 1	Storing at 80 deg.C for 200h	Cold storage at 0 deg.C for 24 hr
				Average transmittance of 400-630 nm light	52.55％	52.30％	53.12％
Average light transmittance of 650-930 nm	0.17％	0.16％	0.17％

Example 2

The embodiment provides a night vision compatible optical filter which is resistant to high and low temperatures and high in visible light transmission, wherein the night vision compatible optical filter is of a laminated structure and comprises a near-infrared absorption layer and an antireflection film layer, and the antireflection film layer is attached to one side of the near-infrared absorption layer; the thickness of the anti-reflection film layer is 60 micrometers, and the thickness of the near-infrared absorption layer is 1 mm; the near-infrared absorption layer and the antireflection film layer have the same expansion coefficient and different refractive indexes.

(1) the same as example 1;

(2) weighing the near-infrared absorbent, chloroform and polymethyl methacrylate according to the mass parts of 0.5, 60 and 40, and sealing and drying the polymethyl methacrylate at the temperature of 80 ℃ for 4 hours;

(3) to (6) the same as in example 1;

table 3: the near-infrared absorption filter of example 2 had average transmittances at room temperature, hot storage and cold storage

Evaluation item	Example 2	Storing at 80 deg.C for 200h	Cold storage at 0 deg.C for 24 hr
				Average light transmittance of 400 nm-630 nm	40.43％	40.43％	40.43％
650 nm-930 nm light average transmittance	0.12％	0.15％	0.13％

Example 3

(1) to (5) the same as in example 1;

(6) weighing polymethyl methacrylate, dodecyl trimethoxy silane, hexafluorobutyl methacrylate, ethyl orthosilicate, lanthanum stearate, stearic acid and nano titanium dioxide according to parts by mass of 40, 15, 20, 15, 8 and 8, uniformly mixing, adding into a reaction container, heating to 60-100 ℃, stirring for reaction for 2.0-4.0 h, and cooling to obtain an anti-reflection protective coating;

table 4: the average transmittance at room temperature, hot storage and cold storage of the near-infrared absorption filter of example 3

Evaluation item	Example 3	Storing at 80 deg.C for 200h	Cold storage at 0 deg.C for 24 hr
				Average light transmittance of 400 nm-630 nm	52.55％	47.78％	42.38％
650 nm-930 nm light average transmittance	0.16％	0.17％	0.16％

Example 4

(1) weighing 15 parts by mass of phthalocyanine dye, 5 parts by mass of anthraquinone dye, 28 parts by mass of methyl phthalocyanine dye, 20 parts by mass of thio-diene type nickel complex dye and 30 parts by mass of o-phenylenediamine type complex dye according to the parts by mass of the near-infrared absorbent, and uniformly mixing;

(2) to (5) the same as in example 1;

(6) weighing polymethyl methacrylate, dodecyl trimethoxy silane, hexafluorobutyl methacrylate, ethyl orthosilicate, lanthanum stearate, stearic acid and nano titanium dioxide according to parts by mass of 40, 15, 5 and 10, uniformly mixing, adding into a reaction container, heating to 60-100 ℃, stirring for reaction for 2.0-4.0 h, and cooling to obtain an anti-reflection protective coating;

table 5: the average transmittance at room temperature, hot storage and cold storage of the near-infrared absorption filter of example 4

Evaluation item	Example 4	Storing at 80 deg.C for 200h	Cold storage at 0 deg.C for 24 hr
				Average light transmittance of 400 nm-630 nm	40.22％	39.14％	41.03％
650 nm-930 nm light average transmittance	0.72％	1.01％	0.72％

And (3) performance detection: spectral transmission tests were performed on the near-infrared absorption filter prepared in comparative example 1 and the night vision compatible filters prepared in examples 1 to 4, respectively, and the results are shown in fig. 2 to 6. As can be seen from a spectrogram, the optimal formula is shown in example 1, the optical filter obtained by the high-low temperature near infrared absorption resistant night vision compatible material has good cut-off performance on light rays with the wave band ranging from 650nm to 900nm, the average transmittance of the optical filter is only 0.2%, the transmittance of the optical filter with the transmittance of 400nm to 630nm in the visible light region reaches more than 50%, and the optical filter still keeps excellent effects in high-low temperature environments. Note: the small graphs in FIGS. 2 to 6 are enlarged graphs of 640 to 900nm wavelength bands.

The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.

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Night vision compatible optical filter resistant to high and low temperatures and high in visible light transmittance and preparation method

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