CN113050212A - Infrared band-pass filter, preparation method thereof and imaging device with infrared band-pass filter - Google Patents
Infrared band-pass filter, preparation method thereof and imaging device with infrared band-pass filter Download PDFInfo
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- CN113050212A CN113050212A CN202110035788.XA CN202110035788A CN113050212A CN 113050212 A CN113050212 A CN 113050212A CN 202110035788 A CN202110035788 A CN 202110035788A CN 113050212 A CN113050212 A CN 113050212A
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- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
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- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
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Abstract
The invention provides an infrared band-pass filter, a preparation method thereof and imaging equipment with the infrared band-pass filter. The infrared band pass filter includes: an absorbing layer (20), the absorbing layer (20) containing a visible light absorbing material; a surface hardening layer (30) provided at least on one side surface of the absorption layer; the light transmittance of the infrared band-pass filter in the wavelength range of 350-700nm is less than or equal to 1 percent; and the light transmittance in the wavelength range of 850-1100nm is greater than or equal to 80%. The infrared band-pass filter is an absorption type infrared band-pass filter, the half-peak value of the transmittance curve of the infrared band-pass filter cannot drift along with incident large-angle light under different incident light angles, and the requirement of an infrared camera on the large-angle drift value of the infrared band-pass filter can be met; and the product can achieve the excellent stability and reliability of 1000 hours of high-temperature high-humidity aging test and the UV irradiation 300-hour cut-off and light transmission variation range of less than 0.5 percent.
Description
Technical Field
The invention relates to the technical field of optics, in particular to an infrared band-pass filter, a preparation method thereof and imaging equipment with the infrared band-pass filter.
Background
The infrared sensing system forms an image by receiving infrared rays reflected by a target, and then obtains information of the target by processing the image, and is generally applied to the fields of face recognition, gesture recognition, smart home and the like. The infrared sensing system comprises a lens, an infrared band-pass filter, an image sensor and the like. The imaging quality of the infrared sensing system can be influenced by the passband change of the infrared bandpass filter under various environmental conditions (such as temperature and ultraviolet rays), and the sensitivity of the infrared sensing system can be influenced by the influence of the incident angle of light on the shift of the center wavelength of the passband. The infrared band-pass filter is a key component of an infrared sensing system, is used for selecting an optical device with a required optical band, and is widely applied to imaging equipment such as mobile phones, cameras, night vision, automatic driving and the like.
An infrared band-pass filter for preventing the semiconductor sensor from influencing UV and visible light noise, and an optical component for cutting off visible light and passing infrared light; at present, there are two main techniques for the optical filter with such performance, one is an interference technique, which generally uses various deposition techniques such as PVD, CVD and the like to enable the optical signal of the target wavelength band based on the multilayer film interference principle to pass through the substrate, and the noise light of the wavelength band outside the target is reflected. The method has the advantages of high transmittance, good reliability, etc. However, as shown in fig. 1, the disadvantage is that the band-pass effect is deteriorated and the noise signal light is incident when the light incidence angle is changed and the interference distance of light propagation is changed, and the deposition process is a vacuum process, and the production control process is complicated and the cost is high.
On the other hand, the absorption technology is adopted, and the absorption type infrared band-pass filter has the advantages that various incident angles can stably maintain the band-pass characteristics, and in addition, the coating process is relatively simple; the defects are that the transmittance of the transmission waveband is slightly low, and the reliability, particularly the UV resistance and the high and low temperature cold and hot shock resistance effect are poor; and the absorption type product obtained by mixing and sintering the heavy metal oxide and the substrate material does not have environmental protection. The invention is achieved accordingly.
Disclosure of Invention
The invention mainly aims to provide an infrared band-pass filter, a preparation method thereof and imaging equipment with the infrared band-pass filter, and aims to solve the problems in the prior art: 1) the infrared band-pass filter prepared by the coating method has the advantages that the optical transmittance curve of the infrared band-pass filter can generate light cut-off drift along with the change of the incident angle of incident light; 2) the absorption infrared band-pass filter is difficult to pass UV and high and low temperature cold and heat shock tests, and the material does not have the problem of environmental protection.
In order to achieve the above object, according to one aspect of the present invention, there is provided an infrared band-pass filter including:
an absorbing layer containing a visible light absorbing material;
the surface hardening layer is at least arranged on one side surface of the absorption layer;
the light transmittance of the infrared band-pass filter in the wavelength range of 350-700nm is less than or equal to 1 percent; and the light transmittance in the wavelength range of 850-1100nm is greater than or equal to 80%.
Further, the infrared band pass filter also has the following transmittance characteristics:
in the range of 560-800 nm of light wavelength, the wavelength value corresponding to the point with the transmittance of 50% in the spectrum is measured when the incident direction of light is vertical to the infrared band-pass filter; the absolute value of the difference of the wavelength values corresponding to the point with the transmittance of 50% in the measurement spectrum when the incident direction of light is incident with an angle of deflection of 35 degrees relative to the vertical direction of the infrared band-pass filter is less than 10 nm;
preferably, in the range of light wavelength 560-800 nm, the light incidence direction is perpendicular to the corresponding wavelength value of 50% transmittance point in the spectrum measured by the infrared band-pass filter; the absolute value of the difference of the wavelength values corresponding to the point with the transmittance of 50% in the measurement spectrum when the incident direction of light is incident with an angle of deflection of 35 degrees relative to the vertical direction of the infrared band-pass filter is less than 5 nm;
preferably, the light transmittance of the infrared band-pass filter in the wavelength range of 350-700nm is less than or equal to 1%; and the light transmittance in the wavelength range of 850-1100nm is more than or equal to 85 percent;
preferably, under the ultraviolet irradiation condition with the wavelength range of 290-390 nm, when the aging time is controlled to be more than 100 hours, in the range of 560-800 nm of the light wavelength, the shift absolute value of the wavelength value of the point corresponding to the point with the transmittance of 50% in the spectrum measured when the incident direction of the light is vertical to the infrared band-pass filter is less than 10 nm;
preferably, under the storage conditions of 85 ℃ of temperature and 85% of relative humidity, when the aging time is controlled to be more than 100 hours, in the range of 560-800 nm of light wavelength, the shift absolute value of the wavelength value of a point corresponding to a point with 50% transmittance in the spectrum is less than 10nm when the incident direction of light is perpendicular to the infrared band-pass filter;
preferably, the infrared band pass filter further includes:
the substrate layer is arranged on the surface of the non-surface hardening layer side of the absorption layer; the substrate layer, the absorption layer and the surface hardening layer are sequentially laminated;
preferably, the visible light absorbing material is selected from a plurality of squarylium organic dyes, phthalocyanine organic dyes, nitrobenzophenone dyes, aminoketone dyes, anthraquinone dyes, quinoline dyes, triazine dyes, benzothiazole dyes and coumarin dyes, iron chromium inorganic dyes, cobalt copper inorganic dyes and chromium inorganic dyes.
The substrate layer (10) is selected from optical glass, organic glass or an organic transparent material;
preferably, the light transmittance of the substrate layer in the wavelength range of 700-1000nm is more than 90%;
preferably, the optical glass comprises sapphire glass, quartz glass, flint glass, crown glass, sodium-boron glass, silicon-aluminum glass, and glass containing lanthanum, barium, phosphorus and lead;
preferably, the organic transparent material is selected from acrylic organic glass, a transparent PC board, a PET material, a cyclic polyolefin layer or a polyimide layer;
preferably, the thickness of the base material layer (10) is 20mm-0.1 mm; preferably, the thickness of the infrared band-pass filter is 3-0.1 mm.
Further, the weight content of the visible light absorption material in the absorption layer is 0.0001-5%, preferably 0.001-2%.
Further, the surface hardening layer is made of organic silicon resin, acrylic resin and polyurethane resin;
the surface hardening layer is formed by photocuring a hardening material composition comprising 40-80 parts by weight of a monomer, 30-80 parts by weight of a diluting solvent, 0.1-5 parts by weight of a functional filler and 0.1-5 parts by weight of an initiator;
preferably, the monomer is selected from one or more of acrylic monomers, polyurethane monomers and amide monomers, preferably the acrylic monomers include acrylate, methacrylic acid derivatives, modified epoxy acrylate, urethane acrylate and aromatic urethane acrylate, more preferably the acrylic monomers are one or more of trimethylolpropane triacrylate, trimethylolpropane trimethacrylate, ethoxylated trimethylolpropane triacrylate, glycerol-propoxylated triacrylate, dihydroxypropyl acrylate, isobornyl methacrylate, 2-ethylhexyl methacrylate and p-neopentyl glycol diacrylate;
preferably, the polyurethane monomer comprises a polyurethane monomer, an acrylic acid modified polyurethane monomer and an epoxy resin modified polyurethane monomer, and more preferably, the polyurethane monomer is one or more of a mixture of polyurethane and octyl acrylate, aromatic urethane acrylate, cresol novolac epoxy acrylate, bisphenol A diacrylate resin and polyurethane arylamine;
preferably, the amide monomers comprise acrylamide chemicals, methacrylamide compounds, amino acid amide compounds and styrene compounds; the diluting solvent is selected from any one or more of ketones, alcohols and esters;
preferably, the diluting solvent is selected from any one or more of butanone, pentanone, cyclopentanone, cyclohexanone, methyl isobutyl ketone, methyl ethyl ketone, methyl isopropyl ketone, ethanol, butanol, ethylene glycol, benzyl alcohol, ethyl acetate, butyl acetate, ethyl acetate, butyl ester, toluene and xylene;
the functional filler comprises oxides having different refractive indices, preferably compounds having a refractive index in the range of 1.3 to 2.8, more preferably any of silica, alumina, silicon monoxide, lanthanum fluoride, yttrium fluoride, barium fluoride, aluminum fluoride, cryolite, titanium dioxide, trititanium pentoxide, titanium sesquioxide, titanium monoxide, hafnium oxide, zirconium oxide, zinc oxide, cerium oxide, zinc sulfide and zinc selenide;
the initiator is selected from any one or more of benzophenone, 1-hydroxy-cyclohexyl ketone, 2-dimethoxy-1, 2-diphenylethanone, benzophenone, 2-hydroxy-2-methyl-1-phenyl acetone, phenyl benzophenone, isopropyl thioxanthone, methyl benzoylformate and 2,4, 6-trimethylphenyl diphenylphosphine oxide.
Further, the infrared band-pass filter also comprises a bottom coating layer arranged between the substrate layer and the absorption layer; the base coat is used for enhancing the bonding force between the base material layer and the absorption layer.
Further, the resin material adopted by the absorption layer is selected from any one of epoxy resin, organic silicon resin, acrylic resin, polyurethane and PU resin.
Another objective of the present invention is to provide an imaging device, which includes an infrared band-pass filter, where the infrared band-pass filter is the infrared band-pass filter.
Another objective of the present invention is to provide an optical sensing system, which includes an image sensor and the infrared band-pass filter, where the infrared band-pass filter is disposed on a light-sensing side of the image sensor.
Another object of the present invention is to provide a method for manufacturing an infrared band-pass filter, which includes the following steps:
s1, stirring and mixing raw materials including the resin material and the visible light absorption material to obtain a coating liquid;
s2, coating the coating liquid on a substrate, and drying to obtain an absorption layer formed by the coating liquid;
and S3, forming a surface hardening layer on at least one side of the absorption layer.
Further, the method may further include the step of previously forming an undercoat layer on the substrate.
The technical scheme of the invention is applied to provide the infrared band-pass filter which comprises an absorption layer, wherein the absorption layer contains a visible light absorption material; the surface hardening layer is at least arranged on one side surface of the absorption layer; the light transmittance of the infrared band-pass filter in the wavelength range of 350-700nm is less than or equal to 1 percent; and the light transmittance in the wavelength range of 850-1100nm is more than or equal to 80 percent, and the absorption layer of the infrared band-pass filter is provided with the visible light absorption material, so that the 50 percent transmittance of the light transmittance curve of the infrared band-pass filter does not drift along with the incident large-angle light, and the curve drift of the infrared band-pass filter is very small under the irradiation of incident light at different angles, thereby meeting the requirement of camera manufacturers on the large-angle drift value of the infrared band-pass filter. On the other hand, the infrared band-pass filter has the advantage that at least one side of the absorption layer is provided with the hardened layer, so that the product can achieve the excellent stability and reliability of 1000 hours of a high-temperature high-humidity aging test and a 300-hour cutoff and light transmission change range of less than 0.5 percent of UV irradiation.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention will be described in further detail below with reference to the drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 shows a transmittance-wavelength relationship curve of a conventional interference-type infrared band-pass filter in the prior art after the optical curves of the filter at different incident light angles.
Fig. 2 is a schematic cross-sectional view illustrating an infrared band-pass filter according to an embodiment of the present invention;
fig. 3 is a schematic cross-sectional view illustrating an infrared band-pass filter according to an embodiment of the present invention;
fig. 4 is a schematic cross-sectional view illustrating an infrared band-pass filter according to an embodiment of the present invention;
fig. 5 is a schematic cross-sectional view illustrating an infrared band-pass filter according to an embodiment of the present invention; and
FIG. 6 is a graph showing a relationship between transmittance and wavelength of an infrared band-pass filter according to an optical curve of the infrared band-pass filter manufactured according to the present invention at different incident light angles;
FIG. 7 is a graph showing a relationship between transmittance and wavelength of an optical curve of the infrared band-pass filter according to the present invention at an incident light angle of 0 ° for different ultraviolet aging times;
fig. 8 is a graph showing the relationship between transmittance and wavelength after an optical curve at an incident light angle of 0 ° under different aging times in high-temperature and high-humidity storage of the infrared band-pass filter manufactured by the present invention.
Wherein the figures include the following reference numerals:
10. a substrate layer; 20. an absorbing layer; 30. a surface hardening layer; 40. and (4) a base coat.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
In order to make the technical solutions of the present invention better understood, 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.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged under appropriate circumstances in order to facilitate the description of the embodiments of the invention herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
As described in the background, the infrared band pass filter in the prior art has the problems of cut-off drift of incident light with large angle and UV aging reliability of the conventional absorption type infrared band pass filter. The inventors of the present invention have studied the above problems and have proposed an infrared band pass filter, comprising an absorption layer 20, wherein the absorption layer 20 contains a visible light absorbing material; and a surface hardening layer 30 disposed at least on one side surface of the absorption layer. The light transmittance of the infrared band-pass filter in the wavelength range of 350-700nm is less than or equal to 1 percent; and the light transmittance in the wavelength range of 850-1100nm is greater than or equal to 80%.
The infrared band-pass filter is an absorption type infrared band-pass filter, and the filter absorption layer is provided with the visible light absorption material, so that the curve left side of the infrared band-pass filter does not drift along with incident large-angle light, and the curve drift of the infrared band-pass filter is very small under the irradiation of incident light at different angles, and the requirement of camera manufacturers on the large-angle drift value of the infrared band-pass filter can be met. In addition, in a preferred scheme of the invention, the visible light absorption material has the property of overlapping absorption spectra, the overlapping absorption spectra of the visible light absorption material can absorb visible light, the transmittance of the visible light is reduced to be less than 1%, and in the wavelength range of 560-800 nm, the corresponding wavelength value of the transmittance of 50% of the transmittance spectrum of the optical filter is measured for the incident light along the normal line relative to the normal line of the optical filter; when the transmittance spectrum of the filter is measured with respect to incident light at an angle of 35 DEG to the normal, the absolute value of the difference between the corresponding wavelength values at which the transmittance is 50% is less than 10 nm. The infrared band-pass filter has excellent ultraviolet and visible light cut-off effects, and the near-infrared band keeps good light transmittance.
On the other hand, the infrared band-pass filter is provided with a special surface hardening layer, the surface hardening layer and the absorption layer are both made of organic resin, and the combination performance of the surface hardening layer and the absorption layer is good. After the product is aged under the condition of 85 ℃/85% RH, comparing the performance change of the product before and after aging, judging by a Baige knife method after a high-temperature high-humidity aging test for 1000 hours and UV irradiation for 300 hours, compared with the product before the aging test, the adhesion force of the surface hardening layer and the absorption layer is kept excellent, and the surface film layer is not dropped. And the light transmittance of the full spectrum is measured, and the fluctuation variation range of the ultraviolet visible light range and the near infrared light transmission range of the light transmittance cut-off is less than 0.5 percent.
Because the surface hardening layer protects the absorption layer to form a functional layer, the oxidation resistance, the UV resistance, the water boiling resistance and the solvent resistance of the absorption layer are improved, the surface hardening layers are mainly organic silicon resin, acrylic resin and polyurethane resin, and some auxiliary agent fillers can be added to improve the oxidation resistance and the UV resistance of the surface hardening layers, so that the optical filter can achieve the excellent performances of high-temperature high-humidity aging test for 1000 hours, UV irradiation for 300 hours and the light transmission change range of less than 0.5%.
In the infrared band-pass filter, the visible light absorption material can absorb light rays in any wave band within the range of 380nm to 750nm, so that the phenomenon that a curve is fixed and the phenomenon that a cut-off curve drifts due to large-angle incident light is prevented. In order to effectively prevent the phenomenon of the shift of the cut-off curve due to the incident light with a large angle, the weight content of the visible light absorbing material in the substrate layer 10 is preferably 0.0001 to 5%, and more preferably 0.001 to 2%.
Preferably, the visible light absorbing material is selected from a plurality of squarylium organic dyes, phthalocyanine organic dyes, nitrobenzophenone dyes, aminoketone dyes, anthraquinone dyes, quinoline dyes, triazine dyes, benzothiazole dyes and coumarin dyes, iron-chromium inorganic dyes, cobalt-copper inorganic dyes and chromium inorganic dyes. The visible light absorption material can not only superpose absorption spectrums to cut off visible light, but also play a role in preventing a light transmittance curve from drifting leftwards under the condition of a large visual angle and preventing the curve from drifting under the condition of large-angle irradiation.
More preferably, the above substrate layer 10 is optical glass, organic glass, or a transparent organic material such as acryl organic glass, a transparent PC plate, a PET plate, a cyclic polyolefin layer (COP), or a transparent polyimide layer (PI). Optical glass can be used as a preferable substrate material, has high light transmittance, and is commonly used in infrared sensing systems. The cyclic polyolefin layer (COP) or the transparent polyimide layer (PI) has not only high toughness and mechanical properties, but also excellent compatibility with the above-mentioned preferred kinds of visible light absorbing materials, both COP and PI materials, and is not easily precipitated.
In the infrared band-pass filter of the present invention, the infrared band-pass filter with various thicknesses can be made according to the thickness of the substrate layer, preferably, the thickness of the substrate layer 10 is 20mm to 0.1mm, at this time, the total thickness of the infrared band-pass filter product is 20mm to 0.11mm, and the thickness of the commercially available infrared band-pass filter is usually 3mm to 0.1mm, that is, the infrared band-pass filter with the visible light absorbing material in the present invention has no influence on the thickness.
In the infrared band-pass filter, the substrate layer of the infrared band-pass filter adopts optical glass, so that the mechanical property of the infrared band-pass filter can be improved, and the scratch resistance of the infrared band-pass filter can be effectively improved. On the other hand, the surface hardening layer on the outer side of the absorption layer 20 can enhance the protection of the absorption layer, and the absorption layer 20 is prevented from being influenced in the reliability test. Preferably, a primer layer 40 is further disposed between the substrate layer and the absorption layer, and when the optical glass is used as the substrate layer, the primer layer may be a silane coupling agent, and the substrate layer and the absorption layer are tightly bonded. After the product is aged under the condition of 85 ℃/85% RH, comparing the performance change of the product before and after aging, judging by a Baige knife method after the high-temperature high-humidity aging test is carried out for 1000 hours and the UV irradiation is carried out for 300 hours, compared with the product before the aging test, the adhesive force between the base material layer 10 and the absorption layer 20 is kept excellent, and the surface film layer is not peeled off.
Preferably, the resin material used for the absorption layer includes acrylic resin and/or methyl isobutyl ketone, and the like.
According to another aspect of the present invention, there is provided an imaging apparatus, including an infrared band-pass filter, and the infrared band-pass filter is the above infrared band-pass filter. The infrared band-pass filter comprises the visible light absorption material arranged in the absorption layer, so that the left side of the curve of the infrared band-pass filter does not drift along with incident large-angle light, the curve drift is very small under the irradiation of the incident light at different angles, and the requirement of mobile phone manufacturers on the large-angle drift value of the infrared band-pass filter can be met. In addition, due to the design of the surface hardening layer, the reliability of the infrared band-pass filter is excellent, the filter can achieve the excellent performance that the high-temperature high-humidity aging test is 1000 hours, the UV irradiation is 300 hours, the cut-off and light transmission change range is less than 0.5%, and the adhesive force of the film layer also meets the requirements of a hundred-fold test.
According to another aspect of the present invention, there is also provided a method for manufacturing an infrared band-pass filter, including the steps of: s1, stirring and mixing raw materials including the resin material and the visible light absorption material to obtain a coating liquid; s2, coating the coating liquid on the substrate layer 10, drying and peeling off to obtain the absorbing layer 20 formed of the coating liquid; s3, forming a surface hardening layer 30 on at least one side of the absorption layer 20, and the structure of the prepared infrared band pass filter is shown in fig. 2.
In a preferred embodiment, the coating liquid is coated on one surface of the substrate layer 10 in the above step S2, dried and not separated to form the absorption layer 20 stacked in the substrate 10, and then the surface hardening layer 30 is formed on one surface of the absorption layer 20, and the structure of the prepared infrared band pass filter is as shown in fig. 3.
The infrared bandpass filter prepared by applying the coating liquid on the other side surface of the substrate layer 10 in the above step S2, drying, and without separation, forming the second layer of the absorption layer 20 stacked in the substrate 10, and then forming the second layer of the surface hardening layer 30 on one side surface of the absorption layer 20 is structured as shown in fig. 5.
Prior to the above step S2, an undercoat layer 40 may be formed on the substrate layer in advance for increasing the adhesion between the substrate layer and the absorption layer, and the structure of the prepared infrared bandpass filter is shown in fig. 4.
In the preparation method of the invention, the base material layer material, the solvent, the visible light absorbing material and the thermosetting initiator can be stirred together to obtain the coating liquid, or the base material layer material and the solvent can be stirred firstly to obtain the mixed liquid, then the visible light absorbing material is added into the mixed liquid and stirred until being dissolved to obtain the coating liquid, the coating liquid is coated on the glass substrate to obtain a wet film, the thickness of the wet film of the coating liquid is 5-250 μm, then the wet film is heated, cured and dried, and the dried coating liquid layer is stripped or not stripped, so that the absorbing layer 20 formed by the coating liquid layer is obtained. By adopting the mode, the visible light absorption material can be better compatible with the material of the base material layer 10, and the visible light absorption material is not separated out. On the other hand, the visible light absorption material can be uniformly dispersed by adopting a thermosetting mode, the film is formed uniformly, and the reliability of the product after high temperature, high humidity and ultraviolet irradiation is better. The visible light absorbing material is arranged on the absorbing layer 20, so that the band pass of the light transmittance curve of the infrared band-pass filter does not drift along with incident large-angle light, the curve drift of the infrared band-pass filter is very small under the irradiation of incident light at different angles, and the requirement of mobile phone manufacturers on the large-angle drift value of the infrared band-pass filter can be met.
In a specific production process, the substrate can be inspected and cleaned to remove dust, colloidal particles, oxides and precipitated substances on the surface, and the substrate is well protected for later use after being cleaned; if necessary, the base plate can be coated with a bottom layer or a film, and various coupling agents can be coated; the coating method can be roll coating, knife coating, slit coating, spin coating, silk screen printing, flexographic printing and the like.
Mixing the visible light absorption material, fully mixing the absorption material with resin, heating and stirring, and filtering for later use; the substrate may be coated with an absorber layer by: the method comprises the following steps of roller coating, blade coating, slit coating, spin coating, screen printing, flexographic printing and the like, and preferably achieves better surface effect through the slit coating and the spin coating. The coated material is cured by thermal curing.
Then forming a surface hardening layer, adding an auxiliary agent into the hardening resin to improve the oxygen resistance, the UV resistance and the high temperature resistance of the hardening resin, stirring and filtering, and adding a cross-linking agent to improve the solvent resistance of the hardening resin; the material of the surface hardening layer is coated by: the method comprises the following steps of roller coating, blade coating, slit coating, spin coating, screen printing, flexographic printing and the like, and preferably achieves better surface effect through the slit coating and the spin coating. The surface hardening layer material may be cured by heat or light, and the light curing is recommended in consideration of solvent resistance.
The visible light absorbing material can absorb light rays in any wave band within the range of 380nm to 450nm, has the transmittance of 50 percent, does not drift at a large visual angle, and prevents the phenomenon of drift of a cut-off curve caused by large-angle incident light. In order to effectively prevent the phenomenon of the shift of the cut-off curve due to the incident light with a large angle, the weight content of the visible light absorbing material in the substrate layer 10 is preferably 0.0001 to 5%, and more preferably 0.001 to 2%. The visible light absorption material can cut off the visible light, so that the transmittance curve of the infrared band-pass filter in a blue light wave band is fixed and does not drift along with the change of incident light angles.
The following will further illustrate the infrared band pass filter and the preparation method thereof provided by the present invention with reference to the following examples.
Example 1 (Silicone series)
The infrared band pass filter provided by the embodiment comprises an absorption layer 20, wherein the absorption layer 20 contains a visible light absorption material; and a surface hardening layer 30 disposed at least on one side surface of the absorption layer.
Wherein the base material layer 10 is a transparent substrate, the material of the transparent substrate is optionally quartz glass, high borosilicate glass, etc., and specifically can be K9, BK70, D263T, AF32, EagleXG, H-ZPK5, H-ZPK7, etc. For example, the substrate layer 10 may be a transparent sheet, and the up-down direction in fig. 2 is a thickness direction of the transparent sheet, and the upper side and the lower side of the transparent sheet are opposite to each other.
The preparation method of the infrared band-pass filter comprises the following steps: adding two-component organic silicon resin OE-6560 (Tao chemical industry) and toluene in a weight ratio of 1:1, uniformly mixing, stirring to obtain a transparent colorless liquid, adding WT =1% visible light absorber IRW3-1 (commercially available from Suzhou group Ye New Material science and technology Co., Ltd.), stirring for 1h to completely dissolve to obtain an absorbing layer coating liquid, standing or vacuum defoaming the coating liquid, coating the coating liquid on a K9, BK70, D263T glass substrate by using a slit coating process, and drying in an oven at 180 ℃ for 2h to obtain an absorbing layer formed by the coating liquid layer, so as to obtain the absorbing layer containing the substrate layer K9, BK70, D263T and the visible light absorbing material with the thickness of 10 mu m.
Coating and hardening on one side surface of the absorption layer, mixing and stirring for one hour by adopting EA6052 (from the Dow chemical industry) and methylbenzene (from the Chinese medicinal chemical Co., Ltd.), coating the absorption layer by using a slit, and drying at 100 ℃; obtaining a surface hardening layer, thus obtaining the product.
Example 2 (acrylic coated organic substrate)
The infrared band pass filter provided by the embodiment comprises an absorption layer 20, wherein the absorption layer 20 contains a visible light absorption material; and a surface hardening layer 30 disposed at least on one side surface of the absorption layer.
Wherein the substrate layer 10 is the transparent basement, and the material of transparent basement is acrylic organic glass, PC panel, PET panel and membrane material etc. optionally. For example, the substrate layer 10 may be a transparent sheet, and the up-down direction in fig. 2 is a thickness direction of the transparent sheet, and the upper side and the lower side of the transparent sheet are opposite to each other.
The preparation method of the infrared band-pass filter comprises the following steps: a polyol-based acrylic resin A-405 (commercially available from Diese synthetic resins (Zhongshan) Co., Ltd.) 1:1 proportion of cyclohexanone (Chinese medicine chemical industry), adding the materials together, uniformly mixing, stirring to obtain a transparent colorless liquid, adding 1 weight percent of visible light absorbent IRW3-2 (a product sold by Suzhou-shou-Ye new material science and technology Co., Ltd.), stirring for 1h until the visible light absorbent IRW3-2 is completely dissolved to obtain an absorption layer coating liquid, standing or defoaming the coating liquid, coating the coating liquid on an acrylic, PC and PET substrate by using a slit coating process, and then putting the substrate into an oven to be dried for 10 h at 80-120 ℃ (according to the heat-resistant condition of the substrate), so as to form an absorption layer, and obtain the absorption layer containing the substrate and the visible light absorption material with the thickness of 10 microns.
Coating a hardening layer on the absorption layer, adding IRGACURE 184 (BASF) and ethyl acetate solvent with the weight ratio of 60% of resin into CN9006UV curing resin (SAODOMA chemical Co., Ltd.), mixing uniformly, coating the mixture on the surface of the absorption layer by using a slit, drying at 70 ℃ for 2 minutes, and curing at UV 340nm for 1 minute to obtain the product.
Example 3 (acrylic primer coated glass)
The infrared band-pass filter provided by the embodiment comprises a bottom coating layer, an absorption layer 20, and a transparent layer, wherein the absorption layer 20 contains a visible light absorption material; and a surface hardening layer 30 disposed at least on one side surface of the absorption layer.
Wherein the base material layer 10 is a transparent substrate, the material of the transparent substrate is optionally quartz glass, high borosilicate glass, etc., and specifically can be K9, BK70, D263T, AF32, EagleXG, H-ZPK5, H-ZPK7, etc. For example, the substrate layer 10 may be a transparent sheet, and the up-down direction in fig. 2 is a thickness direction of the transparent sheet, and the upper side and the lower side of the transparent sheet are opposite to each other.
Adding a base coat to increase the adhesive force, wherein the base coat is KH550 (Zhengzhou Huamai chemical industry), adding absolute ethyl alcohol (Chinese traditional medicine chemical industry) according to a ratio of 1:9, mixing and stirring uniformly; coating the surface of the base glass by a roller coating method, and drying or airing for later use.
The preparation method of the infrared band-pass filter comprises the following steps: a polyol acrylic resin A-405 (Diegon), 1: adding cyclohexanone (Chinese medicine chemical industry) in a proportion of 1 into the mixture, uniformly mixing, stirring the mixture to obtain transparent colorless liquid, adding 1 wt% of visible light absorbent IRW3-3 (a product sold by Suzhou-shou-Ye new material science and technology Co., Ltd.), stirring the mixture for 1h until the mixture is completely dissolved to obtain an absorption layer coating liquid, standing the coating liquid or defoaming the coating liquid in vacuum, coating the coating liquid on a glass substrate which is primed in advance by using a slit coating process, and then putting the glass substrate into an oven to dry the glass substrate for 10 hours at 120 ℃ to form an absorption layer, thus obtaining the absorption layer containing the substrate and the visible light absorbent material with the thickness of 10 micrometers.
Coating a hardening layer on the absorption layer, adding IRGACURE 184 (BASF) and ethyl acetate solvent with the weight ratio of 60% of resin into CN9006UV curing resin (SAODOMA), uniformly mixing, coating the mixture on the surface of the absorption layer by using a slit, drying at 70 ℃ for 2 minutes, and curing at UV 340nm for 1 minute; thus obtaining the product.
The transmittance-wavelength relationship curves of the above prepared optical substrate under the conditions of 0 ° and 35 ° were respectively measured by a lambda1050 spectrophotometer, especially the substrate sample prepared in example 2, the measurement results are shown in fig. 6, the measured optical transmittance curves are consistent under the irradiation of incident light with different incident angles, while the optical curves measured by spectrophotometry of the existing commercially available interference-type infrared band pass filter under different incident light angles are shown in fig. 1,
from the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects: because the infrared band-pass filter comprises the visible light absorption material arranged in the absorption layer, the left side of the curve of the infrared band-pass filter does not drift along with incident large-angle light, and the curve drift of the infrared band-pass filter is very small under the irradiation of the incident light at different angles, so that the requirement of camera manufacturers on the large-angle drift value of the infrared band-pass filter can be met.
Results of reliability test [1 ]:
1.IRW3-1 QUthe samples V-2, IRW3-1 QUV-2168 hrs, IRW3-1 QUV-2336 hrs, IRW3-1 QUV-2504 hrs, IRW3-1 QUV-2672 hrs, IRW3-1 QUV-2840 hrs and IRW3-1 QUV-21008 hrs were sprayed with water at 60 deg.C by UV-LAB aging machine, and UV 3401.2 mw/cm2Irradiation and aging time are respectively as follows: the spectrograms of 0h,168h 336h,504h,672h,840h and 1008h are shown in FIG. 7, and the transmittance spectrums are basically not shifted; and in the range of the wavelength of 560-800 nm under each aging time, the wavelength value drift absolute value of a point corresponding to the point with the transmittance of 50% in the spectrum measured when the light incidence direction is vertical to the infrared band-pass filter is less than 10 nm.
2, IRW 3-185 ℃ 85% RH-2168 hrs, IRW 3-185 ℃ 85% RH-2336 hrs, IRW 3-185 ℃ 85% RH-2504 hrs, IRW 3-185 ℃ 85% RH-2672 hrs, IRW 3-185 ℃ 85% RH-2840 hrs and IRW 3-185 ℃ 85% RH-21008 hrs respectively in THS high temperature and high humidity storage test (macro extension) at 85 ℃, relative humidity 85%, storage for 0h,168h 336h,504h,672h,840h and 1008h, the spectrum performance is as shown in FIG. 8, and the transmittance spectrum is basically not shifted; and in the range of the wavelength of 560-800 nm under each aging time, the wavelength value drift absolute value of a point corresponding to the point with the transmittance of 50% in the spectrum measured when the light incidence direction is vertical to the infrared band-pass filter is less than 10 nm.
The test result proves that the optical filter has excellent ageing resistance proved by two ageing tests.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An infrared band pass filter, comprising:
an absorbing layer (20), the absorbing layer (20) containing a visible light absorbing material;
a surface hardening layer (30) provided at least on one side surface of the absorption layer;
the light transmittance of the infrared band-pass filter in the wavelength range of 350-700nm is less than or equal to 1 percent; and the light transmittance in the wavelength range of 850-1100nm is greater than or equal to 80%.
2. The infrared bandpass filter according to claim 1,
the infrared band-pass filter also has the following transmittance characteristics:
in the range of 560-800 nm of light wavelength, the wavelength value corresponding to the point with the transmittance of 50% in the spectrum is measured when the incident direction of light is vertical to the infrared band-pass filter; the absolute value of the difference of the wavelength values corresponding to the point with the transmittance of 50% in the measurement spectrum when the incident direction of light is incident with an angle of deflection of 35 degrees relative to the vertical direction of the infrared band-pass filter is less than 10 nm;
preferably, in the range of light wavelength 560-800 nm, the light incidence direction is perpendicular to the corresponding wavelength value of 50% transmittance point in the spectrum measured by the infrared band-pass filter; the absolute value of the difference of the wavelength values corresponding to the point with the transmittance of 50% in the measurement spectrum when the incident direction of light is incident with an angle of deflection of 35 degrees relative to the vertical direction of the infrared band-pass filter is less than 5 nm;
preferably, the light transmittance of the infrared band-pass filter in the wavelength range of 350-700nm is less than or equal to 1%; and the light transmittance in the wavelength range of 850-1100nm is more than or equal to 85 percent;
preferably, under the ultraviolet irradiation condition with the wavelength range of 290-390 nm, when the aging time is controlled to be more than 100 hours, in the range of 560-800 nm of the light wavelength, the shift absolute value of the wavelength value of the point corresponding to the point with the transmittance of 50% in the spectrum measured when the incident direction of the light is vertical to the infrared band-pass filter is less than 10 nm;
preferably, under the storage conditions of 85 ℃ of temperature and 85% of relative humidity, when the aging time is controlled to be more than 100 hours, in the range of 560-800 nm of light wavelength, the shift absolute value of the wavelength value of a point corresponding to a point with 50% transmittance in the spectrum is less than 10nm when the incident direction of light is perpendicular to the infrared band-pass filter;
preferably, the infrared band pass filter further includes:
a base material layer (10) provided on a non-surface hardened layer-side surface of the absorption layer (20); the substrate layer (10), the absorption layer (20) and the surface hardening layer (30) are sequentially laminated;
preferably, the visible light absorbing material is selected from a plurality of squarylium organic dyes, phthalocyanine organic dyes, nitrobenzophenone dyes, aminoketone dyes, anthraquinone dyes, quinoline dyes, triazine dyes, benzothiazole dyes and coumarin dyes, iron chromium inorganic dyes, cobalt copper inorganic dyes and chromium inorganic dyes.
3. The infrared bandpass filter according to claim 2, characterized in that the substrate layer (10) is selected from optical glass, organic glass or organic transparent material;
preferably, the light transmittance of the substrate layer in the wavelength range of 700-1000nm is more than 90%;
preferably, the optical glass comprises sapphire glass, quartz glass, flint glass, crown glass, sodium-boron glass, silicon-aluminum glass, and glass containing lanthanum, barium, phosphorus and lead;
preferably, the organic transparent material is selected from acrylic organic glass, a transparent PC board, a PET material, a cyclic polyolefin layer or a polyimide layer;
preferably, the thickness of the base material layer (10) is 20mm-0.1 mm; preferably, the thickness of the infrared band-pass filter is 3-0.1 mm.
4. The infrared bandpass filter according to claim 1, characterized in that the visible light absorbing material is present in the absorbing layer (20) in an amount of 0.0001 to 5% by weight, preferably 0.001 to 2% by weight.
5. The infrared band pass filter as claimed in claim 1, wherein the surface hardening layer is made of silicone resin, acryl resin, or urethane resin;
the surface hardening layer is formed by photocuring a hardening material composition comprising 40-80 parts by weight of a monomer, 30-80 parts by weight of a diluting solvent, 0.1-5 parts by weight of a functional filler and 0.1-5 parts by weight of an initiator; preferably, the monomer is selected from one or more of organosilicon monomer, acrylic monomer, polyurethane monomer and amide monomer;
preferably, the acrylic monomer comprises acrylate, methacrylic acid derivatives, modified epoxy acrylate, urethane acrylate and aromatic urethane acrylate, more preferably, the acrylic monomer is one or more of trimethylolpropane triacrylate, trimethylolpropane trimethacrylate, ethoxylated trimethylolpropane triacrylate, glycerol-propoxylated triacrylate, dihydroxypropyl acrylate, isobornyl methacrylate, 2-ethylhexyl methacrylate and p-neopentyl glycol diacrylate;
preferably, the polyurethane monomer comprises a polyurethane monomer, an acrylic acid modified polyurethane monomer and an epoxy resin modified polyurethane monomer, and more preferably, the polyurethane monomer is one or more of a mixture of polyurethane and octyl acrylate, aromatic urethane acrylate, cresol novolac epoxy acrylate, bisphenol A diacrylate resin and polyurethane arylamine;
preferably, the amide monomers comprise acrylamide chemicals, methacrylamide compounds, amino acid amide compounds and styrene compounds; the diluting solvent is selected from any one or more of ketones, alcohols and esters;
preferably, the diluting solvent is selected from any one or more of butanone, pentanone, cyclopentanone, cyclohexanone, methyl isobutyl ketone, methyl ethyl ketone, methyl isopropyl ketone, ethanol, butanol, ethylene glycol, benzyl alcohol, ethyl acetate, butyl acetate, ethyl acetate, butyl ester, toluene and xylene; the functional filler comprises oxides having different refractive indices, preferably compounds having a refractive index in the range of 1.3 to 2.8, more preferably any of silica, alumina, silicon monoxide, lanthanum fluoride, yttrium fluoride, barium fluoride, aluminum fluoride, cryolite, titanium dioxide, trititanium pentoxide, titanium sesquioxide, titanium monoxide, hafnium oxide, zirconium oxide, zinc oxide, cerium oxide, zinc sulfide and zinc selenide;
the initiator is selected from any one or more of benzophenone, 1-hydroxy-cyclohexyl ketone, 2-dimethoxy-1, 2-diphenylethanone, benzophenone, 2-hydroxy-2-methyl-1-phenyl acetone, phenyl benzophenone, isopropyl thioxanthone, methyl benzoylformate and 2,4, 6-trimethylphenyl diphenylphosphine oxide.
6. The infrared bandpass filter of claim 1, further comprising an undercoat layer (40) disposed between the substrate layer and the absorbing layer; the base coat is used for enhancing the bonding force between the base material layer and the absorption layer.
7. The infrared bandpass filter according to claim 1, wherein the absorbing layer is made of a resin material selected from any one or more of epoxy resin, silicone resin, acrylic resin, polyurethane, and PU resin.
8. An optical sensing system comprising an image sensor and an infrared band-pass filter according to any of claims 1-7, the infrared band-pass filter being arranged on a light-sensitive side of the image sensor.
9. The preparation method of the infrared band-pass filter is characterized by comprising the following steps of:
s1, stirring and mixing raw materials including the resin material and the visible light absorption material to obtain a coating liquid;
s2, coating the coating liquid on a substrate, and drying to obtain an absorption layer (20) formed by the coating liquid;
and S3, forming a surface hardening layer (30) on at least one side of the absorption layer (20).
10. The production method according to claim 9, characterized by further comprising a step of forming an undercoat layer on the substrate in advance.
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| JP7293316B2 (en) | 2017-03-30 | 2023-06-19 | 株式会社Ｄｎｐファインケミカル | Infrared light transmissive composition |
| CN115246985A (en) * | 2022-08-23 | 2022-10-28 | 金发科技股份有限公司 | Stable infrared-transmitting polycarbonate composition for processing and preparation method and application thereof |
| CN115246985B (en) * | 2022-08-23 | 2023-10-17 | 金发科技股份有限公司 | Processing-stable infrared-transmitting white polycarbonate composition and preparation method and application thereof |
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