WO2022176769A1 - 光学フィルタ、赤外線センサ及び発光装置 - Google Patents
光学フィルタ、赤外線センサ及び発光装置 Download PDFInfo
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- WO2022176769A1 WO2022176769A1 PCT/JP2022/005316 JP2022005316W WO2022176769A1 WO 2022176769 A1 WO2022176769 A1 WO 2022176769A1 JP 2022005316 W JP2022005316 W JP 2022005316W WO 2022176769 A1 WO2022176769 A1 WO 2022176769A1
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- Prior art keywords
- optical filter
- less
- wavelength
- inorganic substance
- wavelength band
- Prior art date
Links
- 230000003287 optical effect Effects 0.000 title claims abstract description 153
- 239000000126 substance Substances 0.000 claims abstract description 102
- 239000000463 material Substances 0.000 claims abstract description 86
- 238000010521 absorption reaction Methods 0.000 claims abstract description 80
- 238000002834 transmittance Methods 0.000 claims abstract description 66
- 239000011159 matrix material Substances 0.000 claims abstract description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 42
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- 239000011358 absorbing material Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 4
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- 238000000034 method Methods 0.000 description 28
- 239000002245 particle Substances 0.000 description 27
- 229910010272 inorganic material Inorganic materials 0.000 description 23
- 229910052751 metal Inorganic materials 0.000 description 23
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- 239000002184 metal Substances 0.000 description 16
- 239000011812 mixed powder Substances 0.000 description 16
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- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 8
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- 239000011777 magnesium Substances 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
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- 229920002493 poly(chlorotrifluoroethylene) Polymers 0.000 description 2
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- 150000004645 aluminates Chemical class 0.000 description 1
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- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
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- 238000003763 carbonization Methods 0.000 description 1
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- 238000003384 imaging method Methods 0.000 description 1
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- 150000002823 nitrates Chemical class 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical class O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 1
- 229910052699 polonium Inorganic materials 0.000 description 1
- HZEBHPIOVYHPMT-UHFFFAOYSA-N polonium atom Chemical compound [Po] HZEBHPIOVYHPMT-UHFFFAOYSA-N 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 229910052705 radium Inorganic materials 0.000 description 1
- HCWPIIXVSYCSAN-UHFFFAOYSA-N radium atom Chemical compound [Ra] HCWPIIXVSYCSAN-UHFFFAOYSA-N 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- CNALVHVMBXLLIY-IUCAKERBSA-N tert-butyl n-[(3s,5s)-5-methylpiperidin-3-yl]carbamate Chemical compound C[C@@H]1CNC[C@@H](NC(=O)OC(C)(C)C)C1 CNALVHVMBXLLIY-IUCAKERBSA-N 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- ANRHNWWPFJCPAZ-UHFFFAOYSA-M thionine Chemical compound [Cl-].C1=CC(N)=CC2=[S+]C3=CC(N)=CC=C3N=C21 ANRHNWWPFJCPAZ-UHFFFAOYSA-M 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/206—Filters comprising particles embedded in a solid matrix
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J5/00—Radiation pyrometry, e.g. infrared or optical thermometry
- G01J5/02—Constructional details
- G01J5/08—Optical arrangements
- G01J5/0801—Means for wavelength selection or discrimination
- G01J5/0802—Optical filters
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/208—Filters for use with infrared or ultraviolet radiation, e.g. for separating visible light from infrared and/or ultraviolet radiation
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/22—Absorbing filters
Definitions
- the present invention relates to optical filters, infrared sensors and light emitting devices.
- infrared sensors have been used, for example, as flame sensors or motion sensors. Such infrared sensors detect the presence of flames or humans by receiving infrared rays having a specific wavelength emitted from flames or humans. However, infrared sensors also detect light components emitted from objects other than the detection target and having wavelengths different from those of the detection target. Therefore, in order to remove light components that cause noise, an infrared sensor uses an optical filter that selectively transmits only infrared rays of a specific wavelength.
- Patent Document 1 a particle-dispersed composite infrared ray containing a resin and inorganic compound particles that are uniformly dispersed in the resin and selectively transmit only a specific wavelength band with respect to infrared rays A bandpass filter is disclosed.
- the conventional technology is characterized by easily manufacturing a band-pass filter with a wide selection range of transmission wavelength bands by selecting a combination of resin and inorganic compound particles.
- resin deteriorates due to exposure to ultraviolet rays. Therefore, with the conventional bandpass filter, there is a risk that the optical characteristics may change over time, and there is a risk that the places where it can be used are limited.
- the present invention has been made in view of such problems of the prior art. It is another object of the present invention to provide an optical filter, an infrared sensor, and a light-emitting device having a matrix made of an inorganic substance and having excellent durability.
- an optical filter comprises a matrix composed of an inorganic substance having a solubility in water of 0.4 g/100 g-H 2 O or less; and a wavelength selective absorbing material.
- the optical filter absorbs light components having wavelengths in any band in the wavelength band of interest from 0.8 ⁇ m to 20 ⁇ m.
- the temperature at which the mass reduction rate of the wavelength selective absorption material becomes 10% by mass is 900° C. or less.
- the apparent density of the optical filters relative to the true density of the matrix is 70% or more.
- the wavelength bandwidth at which the linear transmittance per 1 mm thickness of the optical filter is 30% or more is 50 nm or more.
- An infrared sensor includes the above optical filter.
- a light emitting device includes the above optical filter.
- FIG. 1 is a cross-sectional view schematically showing an example of an optical filter according to this embodiment.
- FIG. 2 is an enlarged cross-sectional view of the optical filter of FIG.
- FIG. 3 is a cross-sectional view schematically showing an example of an infrared sensor according to this embodiment.
- FIG. 4 is a schematic diagram showing an example of a light emitting device according to this embodiment.
- FIG. 5 shows infrared spectra of test samples according to Example 1 and Reference Example 1 measured by a transmission method.
- FIG. 6 is the TG curve of melamine.
- FIG. 7 shows infrared spectra of test samples according to Examples 2 to 6 and Reference Example 2 measured by a transmission method.
- FIG. 8 is an infrared spectrum in which a part of FIG. 7 is enlarged.
- FIG. 9 shows infrared spectra of test samples according to Examples 2, 7 and Reference Example 2 measured by a transmission method.
- FIG. 10 is an enlarged infrared spectrum of a portion of FIG.
- FIG. 11 shows infrared spectra of PTFE powder and PVDF powder measured by the ATR method.
- FIG. 12 is the TG curves of PTFE and PVDF.
- optical filter The optical filter, the infrared sensor, the light emitting device, and the method for manufacturing the optical filter according to the present embodiment will be described in detail below with reference to the drawings. Note that the dimensional ratios in the drawings are exaggerated for convenience of explanation, and may differ from the actual ratios.
- the optical filter 1 of this embodiment comprises a matrix 10 and a wavelength selective absorption material 20, as shown in FIG.
- the matrix 10 is composed of inorganic substances. Therefore, compared with the case of using resin, the matrix 10 is less likely to deteriorate over time, and the optical filter 1 with high infrared transmittance can be obtained.
- the water solubility of the inorganic substance constituting the matrix 10 is 0.4 (g/100 g-H 2 O) or less. Since the solubility of the inorganic substance in water is equal to or less than the above value, the optical filter 1 can be stably used even in a high-humidity environment or an underwater environment.
- the solubility was measured under conditions of 1 atm and 25°C.
- the unit of solubility, “g/100 g-H 2 O”, means the mass of inorganic substance dissolved in 100 g of water.
- the inorganic substance forming the matrix 10 contains at least one metal element selected from the group consisting of alkali metals, alkaline earth metals, transition metals, base metals and semi-metals.
- alkaline earth metals include beryllium and magnesium, in addition to calcium, strontium, barium and radium.
- Base metals include aluminum, zinc, gallium, cadmium, indium, tin, mercury, thallium, lead, bismuth and polonium.
- Metalloids include boron, silicon, germanium, arsenic, antimony and tellurium.
- the inorganic substance preferably contains at least one metal element selected from the group consisting of alkali metals such as lithium, zinc, aluminum and magnesium. As will be described later, the inorganic substances containing these metal elements can easily form the joint portion 12 derived from the inorganic substances by a pressure heating method.
- the inorganic substance constituting the matrix 10 is, for example, at least selected from the group consisting of fluorides, oxides, nitrides, hydroxides, hydroxide oxides, sulfides, borides, carbides and halides of the above metal elements. It preferably contains one compound.
- the inorganic substance more preferably contains the above compound as a main component.
- a main component means that an inorganic substance contains 50 mol% or more of said compounds.
- the inorganic substance preferably contains 80 mol % or more of the above compound, more preferably 90 mol % or more.
- the oxides of metal elements described above may include phosphates, silicates, aluminates and borates in addition to compounds in which only oxygen is bonded to metal elements.
- the inorganic substance constituting the matrix 10 may be a composite anion compound containing the metal element.
- a complex anion compound is a substance containing a plurality of anions in a single compound, and examples thereof include acid fluorides, acid chlorides, and oxynitrides.
- the inorganic substance forming the matrix 10 preferably contains at least one selected from the group consisting of fluorides, oxides and hydroxide oxides. Since such inorganic substances have low solubility in water, the optical filter 1 can be stably used even in a high-humidity environment or an underwater environment.
- fluorides include magnesium fluoride and lithium fluoride.
- oxides include aluminum oxide, zinc oxide, magnesium oxide, cerium oxide and yttrium oxide.
- the matrix 10 may contain a plurality of inorganic particles 11. Each of the plurality of inorganic particles 11 are bonded to each other.
- the inorganic particles 11 may be in point contact with each other, or may be in surface contact in which the surfaces of the inorganic particles 11 are in contact with each other.
- the matrix 10 may include a bonding portion 12 that bonds each of the plurality of inorganic particles 11 . Adjacent inorganic particles 11 are bonded via bonding portions 12, whereby the inorganic particles 11 are three-dimensionally bonded to each other, so that the optical filter 1 with high mechanical strength can be obtained. It is preferable that the bonding portion 12 is in direct contact with the inorganic particles 11 .
- the bonding portion 12 preferably covers at least part of the surface of each of the plurality of inorganic particles 11 , and more preferably covers the entire surface of each of the plurality of inorganic particles 11 .
- the bonding portions 12 may exist between the inorganic particles 11 and the wavelength selective absorption material 20 and between the adjacent wavelength selective absorption materials 20 in addition to between the adjacent inorganic particles 11 .
- the inorganic particles 11 may be made of the same inorganic material as the inorganic material that constitutes the matrix 10 as described above.
- the inorganic substance that constitutes the inorganic particles 11 may be crystalline or amorphous.
- the inorganic substance forming the inorganic particles 11 is preferably crystalline from the viewpoint of gas barrier properties or durability.
- the inorganic substance forming the inorganic particles 11 is preferably amorphous from the viewpoint of light transmittance.
- the inorganic particles 11 are crystalline inorganic particles containing at least one metal element selected from the group consisting of alkali metals, alkaline earth metals, transition metals, base metals and semi-metals. is more preferable.
- the inorganic particles 11 are selected from the group consisting of oxides, nitrides, hydroxides, oxide hydroxides, sulfides, borides, carbides and halides of the above metal elements from the viewpoint of gas barrier properties or durability.
- Crystalline particles containing at least one The inorganic particles 11 are crystalline containing at least one selected from the group consisting of oxides, nitrides, hydroxides, hydroxide oxides, sulfides, borides, carbides and halides of the above metal elements. are more preferably inorganic particles.
- the inorganic particles 11 contain 80 mol % or more of at least one selected from the group consisting of oxides, nitrides, hydroxides, hydroxide oxides, sulfides, borides, carbides and halides of the above metal elements. is preferred, more preferably 90 mol % or more, and even more preferably 95 mol % or more. Note that the inorganic substance may be a single crystal or a polycrystal.
- the average particle diameter of the plurality of inorganic particles 11 is preferably 50 nm or more and 50 ⁇ m or less.
- the average particle diameter of the inorganic particles 11 is 50 ⁇ m or less, the light transmittance of the optical filter 1 is increased.
- the average particle diameter of the inorganic particles 11 is within this range, the inorganic particles 11 are strongly bonded to each other, and the strength of the optical filter 1 can be increased.
- the ratio of pores existing inside the optical filter 1 is 30% or less, as will be described later, so that the strength of the optical filter 1 is increased. becomes possible.
- the average particle diameter of the plurality of inorganic particles 11 is more preferably 30 ⁇ m or less, further preferably 20 ⁇ m or less, and particularly preferably 10 ⁇ m or less. preferable.
- the value of "average particle size” is measured using an observation means such as a scanning electron microscope (SEM) or a transmission electron microscope (TEM), and several to several tens of fields of view. A value calculated as an average value of the particle diameters of the particles observed inside is adopted.
- the shape of the inorganic particles 11 is not particularly limited, but can be spherical, for example. Further, the inorganic particles 11 may be whisker-like (needle-like) particles or scale-like particles. The whisker-like particles or scale-like particles are more contactable with other particles than spherical particles, so that the strength of the entire optical filter 1 can be increased.
- the joint portion 12 preferably contains an amorphous inorganic compound.
- the joint portion 12 may be a portion composed only of an amorphous inorganic compound, or may be a portion composed of a mixture of an amorphous inorganic compound and a crystalline inorganic compound. .
- the joint portion 12 may be a portion in which a crystalline inorganic compound is dispersed inside an amorphous inorganic compound.
- the amorphous inorganic compound and the crystalline inorganic compound may have the same chemical composition, or may have different chemical compositions. may have
- the inorganic particles 11 and the bonding portion 12 contain the same metal element, and the metal element is preferably at least one selected from the group consisting of alkali metals, alkaline earth metals, transition metals, base metals and semi-metals. That is, it is preferable that the inorganic compound forming the inorganic particles 11 and the amorphous inorganic compound forming the bonding portion 12 contain at least the same metal element. Further, the inorganic compound forming the inorganic particles 11 and the amorphous inorganic compound forming the bonding portion 12 may have the same chemical composition or may have different chemical compositions.
- a wavelength selective absorbing material 20 is dispersed within the matrix 10 .
- the wavelength selective absorption material 20 may exist between the adjacent inorganic particles 11 or may exist within the bonding portion 12 . Since the wavelength selective absorption material 20 is dispersed in the matrix 10, it is possible to obtain the optical filter 1 with low dependence on the incident angle of light and high light transmittance even when the incident angle is large. That is, even when the optical filter 1 is irradiated with light from an oblique direction, the optical filter 1 can absorb specific light components and transmit other light components.
- the gas barrier property of the inorganic substance forming the matrix 10 is higher than that of the resin, by dispersing the wavelength selective absorption material 20 in the matrix 10, oxidation of the wavelength selective absorption material 20 can be suppressed. Therefore, materials such as oxidizing agents and reducing agents that are unstable in air can also be used as the wavelength selective absorption material 20 .
- the transmission wavelength may change depending on the angle of incidence of light. It is recommended that the light be transmitted in the vertical direction.
- the wavelength selective absorption material 20 is dispersed in the matrix 10 . Therefore, the transmission wavelength hardly depends on the incident angle, and even if light is incident on the surface of the optical filter 1 from an oblique direction, the transmission wavelength is less affected. Therefore, according to the optical filter 1 according to the present embodiment, there is a possibility that it can be expanded to applications that could not be used with interference filters.
- the absorption material that absorbs the light component having a specific wavelength is dispersed in the glass, so the transmitted wavelength does not easily depend on the incident angle.
- the molding temperature for dispersing the glass in the absorber is high. Therefore, only materials that can withstand such molding temperatures can be used, and the degree of freedom in design is low.
- the wavelength selective absorption material 20 can be dispersed in the matrix 10 by a pressure heating method, so the optical filter 1 can be manufactured at a low temperature. .
- the temperature at which the mass reduction rate of the wavelength selective absorption material 20 becomes 10% by mass is 900°C or less. Since the optical filter 1 can be manufactured at a low temperature, even if the wavelength selective absorption material 20 is a compound with low heat resistance, or a material such as an oxidizing agent or reducing agent that is unstable in air, A wavelength selective absorbing material 20 may be dispersed within the matrix 10 .
- the temperature at which the mass reduction rate becomes 10% by mass may be 600° C. or lower, or may be 300° C. or lower. Moreover, the temperature at which the mass reduction rate becomes 10% by mass may be 100° C. or higher.
- the mass reduction rate can be measured by TG (thermogravimetry).
- the wavelength selective absorption material 20 may absorb light components having wavelengths in any band in the target wavelength band of 0.8 ⁇ m to 20 ⁇ m. Since the wavelength-selective absorption material 20 absorbs such light components, when the optical filter 1 is used in, for example, an infrared sensor, the light components that become noise can be removed.
- the target wavelength band may be 1 ⁇ m or more, 2 ⁇ m or more, 3 ⁇ m or more, 7 ⁇ m or more, or 8 ⁇ m or more. Also, the target wavelength band may be 15 ⁇ m or less, 10 ⁇ m or less, or 6 ⁇ m or less.
- the wavelength-selective absorption material 20 may contain at least one selected from the group consisting of inorganic compounds, organic compounds, and deuterium-substituted compounds in which hydrogen contained in these compounds is replaced with deuterium.
- the inorganic compound may contain at least one selected from the group consisting of hydroxides, nitrates, sulfates, hypophosphites such as calcium hypophosphite, and boric acid.
- Organic compounds include fluorine resins, azo-based metal complexes, triarylmethane-based compounds, cyanine-based compounds, squarylium-based compounds, phthalocyanine-based compounds, dithiolate complex-based dyes, diimmonium salt-based compounds, naphthoquinone-based compounds, anthraquinone-based compounds, and melamine. may contain at least one selected from the group consisting of amino compounds.
- Fluororesins include, for example, polytetrafluoroethylene (PTFE), polychlorotrifluoroethylene (PCTFE), polyvinylidene fluoride (PVDF), polyvinyl fluoride (PVF), perfluoroalkoxy fluororesin (PFA), tetrafluoroethylene-hexafluoroethylene At least one selected from the group consisting of fluoropropylene copolymer (FEP), ethylene-tetrafluoroethylene copolymer (ETFE), and ethylene-chlorotrifluoroethylene copolymer (ECTFE) good.
- the fluororesin may be polyvinylidene fluoride (PVDF) or polytetrafluoroethylene (PTFE). Since these fluororesins are used for general purposes, they are readily available.
- the average particle size of the wavelength selective absorption material 20 may be 500 nm or less. When the wavelength selective absorption material 20 has an average particle size of 500 nm or less, light scattering can be suppressed. Although the lower limit of the average particle size of the wavelength selective absorption material 20 is not particularly limited, the average particle size of the wavelength selective absorption material 20 may be 1 nm or more. The average particle size of the wavelength selective absorption material 20 may be 10 nm or more, or may be 100 nm or more. Also, the average particle size of the wavelength selective absorption material 20 may be 400 nm or less, or may be 300 nm or less.
- the refractive index difference between the material forming the matrix 10 and the material forming the wavelength selective absorption material 20 may be 0.1 or less. When the refractive index difference is 0.1 or less, light scattering can be suppressed.
- the lower limit of the refractive index difference is not particularly limited as long as the refractive index difference is 0 or more.
- the refractive index difference may be 0.01 or more, or 0.02 or more. Also, the refractive index difference may be 0.08 or less, or may be 0.04 or less.
- the apparent density (hereinafter also referred to as "relative density") of the optical filter 1 with respect to the true density of the matrix 10 is 70% or more.
- the relative density is 70% or more, the optical filter 1 becomes dense and the amount of light transmitted through the optical filter 1 increases.
- the relative density is 70% or more, the optical filter 1 becomes denser and its strength increases. Therefore, it is possible to improve the machinability of the optical filter 1 .
- the bending strength of the optical filter 1 can be increased.
- the relative density of the optical filter 1 is more preferably 80% or higher, even more preferably 90% or higher, and particularly preferably 95% or higher.
- the porosity in the cross section of the optical filter 1 is preferably 30% or less. That is, when observing the cross section of the optical filter 1, the average value of the ratio of pores per unit area is preferably 30% or less. If the porosity is 30% or less, the amount of light that passes through the optical filter 1 increases. Moreover, when the porosity is 30% or less, the optical filter 1 becomes denser and the strength increases. Therefore, it is possible to improve the machinability of the optical filter 1 . Further, when the porosity is 30% or less, cracks are suppressed from occurring in the optical filter 1 starting from the pores, so the bending strength of the optical filter 1 can be increased.
- the porosity in the cross section of the optical filter 1 is more preferably 20% or less, even more preferably 10% or less, and particularly preferably 5% or less. The smaller the porosity in the cross section of the optical filter 1, the more the cracks starting from the pores are suppressed, so the strength of the optical filter 1 can be increased.
- the porosity can be obtained as follows. First, the cross section of the optical filter 1 is observed to identify the matrix 10 and pores. Then, the unit area and the area of pores in the unit area are measured, the ratio of pores per unit area is obtained, and the obtained value is taken as the porosity. It is more preferable to calculate the ratio of pores per unit area at a plurality of locations on the cross section of the optical filter 1, and then use the average value of the ratios of pores per unit area as the porosity.
- an optical microscope, a scanning electron microscope (SEM), or a transmission electron microscope (TEM) can be used.
- the unit area and the area of pores in the unit area may be measured by binarizing the image observed with a microscope.
- the size of the pores present inside the optical filter 1 is not particularly limited, it is preferably as small as possible. Since cracks originating from the pores are suppressed by the small size of the pores, the strength of the optical filter 1 can be increased and the machinability of the optical filter 1 can be improved. In addition, since the pore size is small, light scattering is suppressed, so that the transmittance can be increased.
- the pore size of the optical filter 1 is preferably 5 ⁇ m or less, more preferably 1 ⁇ m or less, and even more preferably 100 nm or less. The size of the pores present inside the optical filter 1 can be determined by observing the cross section of the optical filter 1 with a microscope, as with the porosity described above.
- the volume ratio of the plurality of inorganic particles 11 is preferably 30% or more. In this case, the obtained optical filter 1 becomes a structure in which the characteristics of the inorganic particles 11 are easily utilized.
- the volume ratio of the plurality of inorganic particles 11 is more preferably 40% or more, more preferably 50% or more.
- the volume ratio of the inorganic particles 11 is preferably larger than the volume ratio of the joints 12 .
- the volume ratio of the wavelength selective absorption material 20 in the optical filter 1 is preferably 0.1% by volume or more and 30% by volume or less, although it depends on the transmission characteristics of the optical filter 1 and the like.
- the volume ratio of the wavelength selective absorption material 20 is 0.1% by volume or more, the amount of light absorbed by the optical filter 1 can be improved. Further, by setting the volume ratio of the wavelength selective absorption material 20 to 30% by volume or less, the mechanical properties of the optical filter 1 can be improved.
- the volume ratio of the wavelength selective absorption material 20 is more preferably 0.2 volume % or more, and more preferably 0.5 volume % or more. Further, the volume ratio of the wavelength selective absorption material 20 is more preferably 15% by volume or less, even more preferably 10% by volume or less, and particularly preferably 5% by volume or less.
- the optical filter 1 absorbs light components having wavelengths in any band in the target wavelength band of 0.8 ⁇ m to 20 ⁇ m. Since the optical filter 1 absorbs such light components, when the optical filter 1 is used for a sensor or the like, the optical filter 1 can remove light components that become noise.
- the target wavelength band may be 1 ⁇ m or more, 2 ⁇ m or more, or 3 ⁇ m or more. Also, the target wavelength band may be 15 ⁇ m or less, 10 ⁇ m or less, or 6 ⁇ m or less.
- the wavelength bandwidth at which the linear transmittance per 1 mm thickness of the optical filter 1 is 30% or more is 50 nm or more. Since the optical filter 1 has such characteristics, it is possible to transmit a part of the light components while cutting a part of the light components in the target wavelength band. As a result, when the optical filter 1 is used in, for example, an infrared sensor, the optical filter 1 can remove the light component that becomes noise, allowing the light component to be detected to reach the infrared sensor. Therefore, an infrared sensor with little noise and high sensitivity can be obtained.
- the wavelength bandwidth at which the in-line transmittance is 30% or more may be 100 nm or more, 300 nm or more, or 500 nm or more. Also, the wavelength bandwidth at which the in-line transmittance is 30% or more may be 5000 nm or less, 3000 nm or less, or 1000 nm or less. Also, the linear transmittance may be 35% or more, or 40% or more.
- the upper limit of the in-line transmittance is not particularly limited, and is, for example, 100%.
- the wavelength bandwidth at which the linear transmittance per 1 mm thickness of the optical filter 1 is 1% or less is preferably 50 nm or more. Since the optical filter 1 has such characteristics, when the optical filter 1 is used in, for example, an infrared sensor, it is possible to largely cut off light components that become noise. Therefore, an infrared sensor with little noise and high sensitivity can be obtained.
- the wavelength bandwidth at which the in-line transmittance is 1% or less may be 100 nm or more, 300 nm or more, or 500 nm or more.
- the wavelength bandwidth at which the in-line transmittance is 1% or less may be 10000 nm or less, 5000 nm or less, 3000 nm or less, or 1000 nm or less.
- the linear transmittance may be 0.5% or less, or may be 0.2% or less.
- the lower limit of the in-line transmittance is not particularly limited, and is, for example, 0%.
- the wavelength bandwidth at which the in-line transmittance is 30% or more is preferably 300 nm or more.
- the wavelength bandwidth in which the linear transmittance is 1% or less is preferably 300 nm or more.
- the wavelength bandwidth at which the linear transmittance is 30% or more is preferably 300 nm or more, and the wavelength bandwidth at which the linear transmittance is 1% or less is preferably 300 nm or more.
- Optical filters 1 such as these are useful as band-pass filters or band-cut filters.
- the linear transmittance over the entire wavelength band of 8 ⁇ m to 20 ⁇ m may be 10% or less.
- Such an optical filter 1 can be used as a filter for cutting wavelengths in the long wavelength band. Since such a filter can reduce noise in the long wavelength region, erroneous detection can be suppressed when it is used in an infrared sensor, for example. In addition, by cutting such a wide wavelength band, it is possible to increase the degree of freedom in designing devices such as infrared sensors.
- the linear transmittance over the entire wavelength band of 8 ⁇ m to 20 ⁇ m may be 8% or less, 5% or less, 2% or less, or 1% or less.
- the linear transmittance over the entire wavelength band of 7 ⁇ m to 20 ⁇ m may be 10% or less.
- the linear transmittance over the entire wavelength band of 7 ⁇ m to 20 ⁇ m may be 9% or less, 6% or less, 4% or less, or 1% or less.
- the inorganic substance may contain fluoride, and the wavelength selective absorption material 20 may contain fluororesin.
- the optical filter 1 that cuts, for example, wavelengths in the long wavelength band as described above.
- Fluororesin has a C—F bond and absorbs light in the wavelength band of 8 ⁇ m to 9 ⁇ m. Therefore, by combining with the fluoride matrix 10, an optical filter that cuts a specific wavelength in the long wavelength band as described above, for example. 1 can be provided.
- the fluoride those mentioned above can be used, and for example, lithium fluoride may be used.
- the above-described fluorine resin can be used, and for example, polyvinylidene fluoride (PVDF) or polytetrafluoroethylene (PTFE) may be used.
- PVDF polyvinylidene fluoride
- PTFE polytetrafluoroethylene
- PVDF absorbs light components in the wavelength band of 8 ⁇ m to 9 ⁇ m
- PVDF may be used as the fluororesin.
- the linear transmittance can be obtained by measuring the optical filter 1 by a transmission method with an FT-IR (Fourier transform infrared spectroscopy) device.
- the linear transmittance of the infrared transmission spectrum is converted to the linear transmittance at a thickness of 1 mm based on the Beer-Lambert law.
- the wavelength bandwidth can be obtained by measuring the wavelength bandwidth at which the linear transmittance is equal to or greater than or equal to a predetermined value in the target wavelength band.
- the wavelength bandwidth may be a wavelength bandwidth in which the linear transmittance is continuously greater than or equal to a predetermined value or less, and a wavelength bandwidth in which the linear transmittance is continuously and intermittently greater than or equal to or less than a predetermined value may be the total wavelength bandwidth of That is, the wavelength bandwidth is the total wavelength bandwidth in which the linear transmittance is equal to or greater than a predetermined value, or the total wavelength bandwidth in which the linear transmittance is equal to or less than a predetermined value in the target wavelength band. Therefore, when the linear transmittance is intermittently higher or lower than the predetermined value, the wavelength bands in which the linear transmittance is higher than or lower than the predetermined value may be separated from each other in the target wavelength band.
- the wavelength bandwidth is preferably a wavelength bandwidth in which the linear transmittance is continuously equal to or greater than or equal to or less than a predetermined value.
- the wavelength bandwidth in which the linear transmittance per 1 mm thickness of the optical filter 1 is continuously 30% or more may be 50 nm or more.
- the wavelength bandwidth in which the linear transmittance is continuously 1% or less may be 300 nm or more.
- the thickness t of the optical filter 1 is not particularly limited, it can be, for example, 100 ⁇ m or more.
- the optical filter 1 of this embodiment is formed by a pressure heating method, as will be described later. Therefore, an optical filter 1 having a large thickness can be easily obtained.
- the thickness of the optical filter 1 may be 500 ⁇ m or more, 1 mm or more, or 1 cm or more.
- the upper limit of the thickness of the optical filter 1 is not particularly limited, it can be set to 50 cm, for example.
- the optical filter 1 includes a matrix 10 composed of an inorganic substance having a solubility in water of 0.4 (g/100 g-H 2 O) or less, and a wavelength selective absorption material dispersed in the matrix 10. 20.
- the optical filter 1 absorbs light components having wavelengths in any band in the target wavelength band from 0.8 ⁇ m to 20 ⁇ m. In the case of heating in air from 100° C. at a rate of 10° C./min, the temperature at which the mass reduction rate of the wavelength selective absorption material 20 becomes 10% by mass is 900° C. or less.
- the apparent density of the optical filter 1 with respect to the true density of the matrix 10 is 70% or more.
- the wavelength bandwidth at which the linear transmittance per 1 mm thickness of the optical filter 1 is 30% or more is 50 nm or more.
- the optical filter 1 has the matrix 10 made of an inorganic substance, and thus has excellent durability.
- the matrix 10 is composed of an inorganic substance that has a higher gas barrier property than resin, and the wavelength selective absorption material 20 is dispersed within the matrix 10 .
- the relative density of the matrix 10 to the apparent density of the optical filter 1 is high and dense. Therefore, the optical filter 1 according to this embodiment can protect the wavelength selective absorption material 20 from the air existing in the external space. Therefore, it may be possible to use materials with low stability to oxygen or water as the wavelength selective absorption material 20, which have not been available in the past.
- the infrared sensor 100 includes the optical filter 1 described above, as shown in FIG.
- the infrared sensor 100 also includes an infrared detection element 110 , an IC element 120 , a substrate 130 and a metal case 150 .
- the infrared detection element 110 and the IC element 120 are mounted on the substrate 130 with a die bonding material 131 . Infrared detection element 110 and IC element 120 are electrically connected to each other by wire 140 . Also, the infrared detection element 110 is connected to an electric circuit wiring (not shown) of the substrate 130 by a wire 140 .
- the infrared detection element 110 receives infrared rays, converts the thermal energy of the received infrared rays into electrical energy, and outputs an electrical signal corresponding to the amount of received infrared rays to the IC element 120 .
- the infrared detection element 110 may be a pyroelectric element, a thermal infrared detection element such as a thermopile infrared detection element or a bolometer infrared detection element, or a quantum infrared detection element.
- the IC element 120 includes an amplifier circuit that amplifies the electrical signal output from the infrared detection element 110, and a determination circuit that determines that a flame exists when the electrical signal amplified by the amplifier circuit exceeds a threshold value. .
- the metal case 150 is attached to the substrate 130.
- a metal case 150 surrounds the infrared detection element 110 and the IC element 120 , and the substrate 130 and the metal case 150 hermetically seal the infrared detection element 110 and the IC element 120 .
- Metal case 150 includes a top wall 151 and side walls 152 .
- An opening is provided in the upper wall 151 and the opening is covered with the optical filter 1 .
- Optical filter 1 is arranged to face infrared detection element 110 , and infrared detection element 110 is provided on substrate 130 so as to receive infrared rays that have passed through optical filter 1 .
- a side wall 152 connects the edge of the top wall 151 and the edge of the substrate 130 .
- Infrared rays emitted from a flame or the like pass through the optical filter 1 and are received by the infrared detection element 110 .
- the infrared detection element 110 outputs an electric signal to the IC element 120 according to the amount of received infrared rays.
- IC element 120 determines whether a flame is present in response to the electrical signal.
- the infrared sensor 100 can detect flames using infrared rays emitted from the flames.
- the infrared sensor 100 is used as a flame sensor for detecting flame has been described, but the application of the infrared sensor 100 is not limited to such a form.
- the infrared sensor 100 can also be used as a human sensor, a biosensor, a security sensor, a gas sensor, a non-contact thermometer, a solid-state imaging device, a camera module, or the like.
- the light emitting device 200 includes the optical filter 1 described above, as shown in FIG.
- the light emitting device 200 also includes a light source 210 that irradiates the optical filter 1 with light containing infrared rays.
- Light source 210 may include LEDs, xenon lamps, laser diodes, and combinations thereof.
- the light-emitting device 200 has the optical filter 1 , part of the infrared rays emitted from the light source 210 can be cut by the optical filter 1 . Therefore, according to the light emitting device 200 according to this embodiment, it is possible to irradiate light having a specific wavelength.
- the light-emitting device 200 can be used, for example, as a light-emitting device for inspection, a light-emitting device for monitoring cameras, a light-emitting device for depilation, a light-emitting device for curing an infrared curable resin, and the like.
- the optical filter 1 can be manufactured by pressurizing and heating a mixture of particles of an inorganic substance and a wavelength selective absorption material containing a solvent. By using such a pressurized heating method, a part of the inorganic substance is eluted and the inorganic substances are bonded to each other, so that the optical filter 1 in which the wavelength selective absorption material 20 is dispersed can be formed.
- an inorganic substance powder and a wavelength selective absorption material powder are mixed to prepare a mixed powder.
- the method of mixing the powder of the inorganic substance and the powder of the wavelength-selective absorption material is not particularly limited, and the mixing can be carried out by a dry method or a wet method. Further, the powder of the inorganic substance and the powder of the wavelength selective absorption material may be mixed in air or in an inert atmosphere.
- a wavelength selective absorption material and a solvent are mixed. The wavelength selective absorption material may or may not be dissolved in the solvent. Then, a mixture containing the inorganic substance, the wavelength selective absorption material, and the solvent may be prepared by adding the powder of the inorganic substance to the mixture of the wavelength selective absorption material and the solvent.
- the solvent is not particularly limited, for example, a solvent capable of partially dissolving the inorganic substance when the mixed powder is pressurized and heated can be used.
- a solvent a solvent that can react with an inorganic substance to produce an inorganic substance different from the inorganic substance can be used.
- a solvent at least one selected from the group consisting of acidic aqueous solutions, alkaline aqueous solutions, water, alcohols, ketones and esters can be used.
- the acidic aqueous solution an aqueous solution with a pH of 1 to 3 can be used.
- an alkaline aqueous solution an aqueous solution with a pH of 10 to 14 can be used.
- the acidic aqueous solution it is preferable to use an aqueous solution of an organic acid.
- the alcohol it is preferable to use an alcohol having 1 to 12 carbon atoms.
- the interior of the mold is filled with a mixture containing an inorganic substance, a wavelength selective absorption material, and a solvent.
- the mold may be heated as necessary. Then, by applying pressure to the mixture inside the mold, the inside of the mold becomes a high pressure state. At this time, the inorganic substance and the wavelength selective absorption material are densified, and at the same time, the particles of the inorganic substance are bonded to each other.
- the inorganic compound that constitutes the inorganic substance dissolves in the solvent under high pressure.
- the dissolved inorganic compound penetrates the voids between the inorganic substance and the wavelength selective absorbing material, the voids between the inorganic substances, and the voids between the wavelength selective absorbing material.
- connecting portions derived from the inorganic substance are formed between the inorganic substance and the wavelength selective absorption material, between the inorganic substances and between the wavelength selective absorption material. .
- the inorganic compound that constitutes the inorganic substance reacts with the solvent under high pressure. Then, the other inorganic substance generated by the reaction fills the gaps between the inorganic substance and the wavelength selective absorption material, the gaps between the inorganic substances, and the gaps between the wavelength selective absorption material, and the other inorganic substance A derived joint is formed.
- the heating and pressurizing conditions for the mixture containing the inorganic substance, the wavelength selective absorption material, and the solvent are such that when a solvent that partially dissolves the inorganic substance is used, the dissolution of the surface of the inorganic substance progresses.
- the heating and pressurizing conditions for the mixture are such that when a solvent that reacts with an inorganic substance to produce an inorganic substance different from the inorganic substance is used as the solvent, the reaction between the inorganic substance and the solvent proceeds.
- the temperature at which the mixture containing the inorganic substance, the wavelength selective absorption material and the solvent is heated is more preferably 80 to 250.degree. C., more preferably 100 to 200.degree.
- the pressure when pressurizing the mixture containing the inorganic substance, the wavelength selective absorption material, and the solvent is more preferably 50 to 600 MPa.
- the optical filter 1 can be obtained by taking out the molded body from the inside of the mold.
- the connecting portion derived from the inorganic substance, which is formed between the inorganic substance and the wavelength selective absorbing material, between the inorganic substance, and between the wavelength selective absorbing material is preferably the above-described connecting portion 12 .
- a sintering method is known as a method for manufacturing inorganic members made of ceramics.
- the sintering method is a method of obtaining a sintered body by heating an aggregate of solid powder made of an inorganic substance at a temperature lower than the melting point.
- the solid powder is heated to, for example, 1000° C. or higher. Therefore, even if an attempt is made to obtain a composite member composed of an inorganic substance and a wavelength-selective absorption material using a sintering method, the wavelength-selective absorption material is carbonized by heating at a high temperature, making it impossible to obtain a composite member.
- the mixture obtained by mixing the powder of the inorganic substance and the powder of the wavelength selective absorption material is heated at a low temperature of 300° C. or less, so that the wavelength selective absorption material is carbonized. Hard to happen. Therefore, the wavelength selective absorption material 20 can be stably dispersed inside the matrix 10 made of an inorganic substance.
- the mixture obtained by mixing the powder of the inorganic substance and the powder of the wavelength selective absorption material is pressed while being heated. Become. As a result, since the number of pores inside the matrix 10 is reduced, it is possible to obtain the optical filter 1 having high strength while suppressing oxidation degradation of the wavelength selective absorption material 20 .
- the method for manufacturing the optical filter 1 includes a step of mixing inorganic substance powder and wavelength selective absorption material powder to obtain a mixture, and adding a solvent that dissolves the inorganic substance or a solvent that reacts with the inorganic substance to the mixture. and then pressurizing and heating the mixture.
- the method for manufacturing the optical filter 1 includes a step of mixing a wavelength selective absorption material into a solvent that dissolves an inorganic substance or a solvent that reacts with the inorganic substance, and mixing powder of the inorganic substance into the solvent containing the wavelength selective absorption material. to obtain a mixture; and pressurizing and heating the mixture.
- the mixture is preferably heated and pressurized at a temperature of 50 to 300° C.
- the optical filter 1 since the optical filter 1 is formed under such low temperature conditions, carbonization of the wavelength selective absorption material 20 is suppressed, and a colored ceramic member can be obtained.
- a solvent that dissolves the inorganic substance or a solvent that reacts with the inorganic substance is added to the mixture.
- the optical filter 1 does not need to add a solvent that dissolves the inorganic substance or a solvent that reacts with the inorganic substance to the mixture. That is, the optical filter 1 may be obtained by pressurizing and heating a mixture obtained by mixing powder of an inorganic substance and powder of a wavelength selective absorption material. For example, when lithium fluoride is used as the inorganic substance, it plastically deforms at high temperatures, so that the dense optical filter 1 can be manufactured by pressing at a temperature higher than the plastically deforming temperature.
- Example 1 First, as inorganic particles, lithium fluoride powder (Fuji Film Wako Pure Chemical Industries, Ltd., special reagent grade) having a solubility in water of 0.134 g/100 mL and an average particle size of 5 ⁇ m was prepared. In addition, melamine powder (Fujifilm Wako Pure Chemical Industries, Ltd., special reagent grade) was prepared as a wavelength selective absorption material. Next, lithium fluoride powder and melamine powder are mixed by adding acetone using an agate mortar and an agate pestle so that the mass ratio is 99:1 (volume ratio is 98.3:1.7). A mixed powder was obtained.
- lithium fluoride powder Fluji Film Wako Pure Chemical Industries, Ltd., special reagent grade
- the mixed powder was put into the inside of a cylindrical molding die ( ⁇ 10) having an internal space. Further, the mixed powder was heated and pressurized under conditions of 180° C., 400 MPa, and 30 minutes. In this way, a cylindrical test sample of this example was obtained.
- test sample was prepared in the same manner as in Example 1 except that no wavelength selective absorption material was added. That is, the lithium fluoride powder used in Example 1 was heated and pressurized in the same manner as in Example 1.
- the in-line transmittance is reduced in several bands, and the wavelength selective absorption material is found to be absorbed. From this, it can be seen that the wavelength selective absorption material remains in the test sample without being decomposed.
- the maximum transmittance of the test sample of Example 1 was 56% at a wavelength of 5.71 ⁇ m. Also, the band where the linear transmittance was 1/2 (28%) of the maximum transmittance was 5.13 ⁇ m to 5.84 ⁇ m, and the full width at half maximum was 705 nm.
- the band in which the in-line transmittance was 30% or more was in the range of 5.21 ⁇ m to 5.83 ⁇ m, and the bandwidth was 621 nm.
- the linear transmittance was continuously about 0.4%, and the wavelength bandwidth was 400 nm.
- the in-line transmittance was intermittently about 0.6%.
- TG thermogravimetry
- melamine began to lose mass at around 240°C, with a mass loss rate of 5% at 279°C and a mass loss rate of 10% at 292°C. From this result, it can be seen that the temperature at which the rate of mass reduction becomes 10% is 300° C. or less when melamine is heated in air at a rate of 10° C./min from 100° C. In this example, the mixed powder is heated and pressed under the conditions of 180° C., 400 MPa, and 30 minutes, so it can be seen that even a material with low heat resistance such as melamine can be dispersed in the inorganic matrix. .
- the relative densities of the test samples of Example 1 and Reference Example 1 were measured. Specifically, first, the volume and mass of the test sample were measured, and the apparent density of the test sample was calculated. Next, the relative density of the test sample was calculated by dividing the apparent density of the test sample by the true density of the matrix lithium fluoride.
- the relative density of the test sample of Example 1 was 89%, and the relative density of the test sample of Reference Example 1 was 90%. That is, the porosity of the test sample of Example 1 is estimated to be 11%, and the porosity of the test sample of Reference Example 1 is estimated to be 10%. From these results, it can be understood that the porosity of the test sample is small and the test sample has a dense structure.
- test samples according to Examples 2 to 7 and Reference Example 2 were prepared and evaluated.
- Example 2 lithium fluoride powder having a water solubility of 0.134 g/100 mL and an average particle diameter of 1 ⁇ m was prepared as inorganic particles. Moreover, PVDF was prepared as a wavelength selective absorption material. Next, the lithium fluoride powder and the PVDF powder were mixed with acetone using an agate mortar and an agate pestle so that the mass ratio was 99:1 (volume ratio 98.5:1.5). , to obtain a mixed powder.
- the lithium fluoride powder was produced as follows. First, 8.9 g of LiCl (Fujifilm Wako Pure Chemical Co., Ltd. Wako special grade) was dissolved in 35 ml of deionized water to prepare a LiCl solution. Also, 12.2 g of KF (Fujifilm Wako Pure Chemical Industries, Ltd. special grade reagent) was dissolved in 35 mL of deionized water to prepare a KF solution. Next, the total amount of LiCl solution and the total amount of KF solution were mixed at room temperature and stirred for 3 minutes with a magnetic stirrer. This stirred liquid was subjected to suction filtration using a membrane filter with a pore size of 0.1 ⁇ m, and the residue was dried to obtain lithium fluoride powder.
- LiCl LiCl
- KF Flujifilm Wako Pure Chemical Industries, Ltd. special grade reagent
- PVDF Sigma-Aldrich's PVDF (average Mw ⁇ 534,000 by GPC, powder) was used.
- the average particle size of PVDF is about 200 nm. Since the refractive index of lithium fluoride is 1.39 and the refractive index of PVDF is 1.42, the difference in refractive index between lithium fluoride and PVDF is 0.03.
- the mixed powder was put into the inside of a cylindrical molding die ( ⁇ 12) having an internal space. Then, the mixed powder was heated and pressurized under conditions of 200° C., 400 MPa, and 10 minutes. In this way, a cylindrical test sample of this example was obtained. The thickness of the test sample was 1053 ⁇ m.
- Example 3 A test sample was prepared in the same manner as in Example 2, except that the mass ratio of the lithium fluoride powder and the PVDF powder in the mixed powder was 98:2 (volume ratio 97.1:2.9). The thickness of the test sample was 1057 ⁇ m.
- Example 4 A test sample was prepared in the same manner as in Example 2, except that the mass ratio of the lithium fluoride powder and the PVDF powder in the mixed powder was set to 97:3 (volume ratio of 95.6:4.4). The thickness of the test sample was 1017 ⁇ m.
- Example 5 A test sample was prepared in the same manner as in Example 2, except that the mass ratio of the lithium fluoride powder and the PVDF powder in the mixed powder was set to 96:4 (volume ratio of 94.2:5.8). The thickness of the test sample was 1014 ⁇ m.
- Example 6 A test sample was prepared in the same manner as in Example 2, except that the mass ratio of the lithium fluoride powder and the PVDF powder in the mixed powder was set to 92:8 (volume ratio of 88.6:11.4). The thickness of the test sample was 1064 ⁇ m.
- Example 7 A test sample was prepared in the same manner as in Example 2, except that PTFE powder (Kitamura KTL-1N, manufactured by Kitamura Co., Ltd.) was used instead of PVDF powder. Specifically, the mass ratio of the lithium fluoride powder and the PTFE powder in the mixed powder was set to 99:1 (volume ratio of 98.4:1.6). The thickness of the test sample was 1147 ⁇ m.
- PTFE powder Kitamura KTL-1N, manufactured by Kitamura Co., Ltd.
- test sample was prepared in the same manner as in Example 2, except that the mass ratio of the lithium fluoride powder and the PVDF powder in the mixed powder was 100:0.
- the thickness of the test sample was 1064 ⁇ m.
- test samples of Examples 2 to 7 had a linear transmittance of 30% or more per 1 mm thickness of the test sample in the target wavelength band of 0.8 ⁇ m to 20 ⁇ m. was 50 nm or more. These results suggested that the test samples of Examples 2 to 7 are useful as optical filters.
- the linear transmittance was 10% or less over the entire wavelength band of 8 ⁇ m to 20 ⁇ m. It was also found that the linear transmittance decreased as the amount of fluororesin added increased. It was also found that the use of PVDF as the fluororesin can lower the linear transmittance in the wavelength band of 7 ⁇ m to 8 ⁇ m compared to the use of the same amount of PTFE. These results suggest that the test samples of Examples 2 to 7 are useful as filters for cutting wavelengths in the long wavelength band.
- TG thermogravimetry
- an optical filter an infrared sensor, and a light-emitting device with excellent durability that include a matrix made of an inorganic substance.
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Abstract
Description
本実施形態の光学フィルタ1は、図1に示すように、マトリックス10と、波長選択吸収材料20とを備えている。
次に、本実施形態に係る赤外線センサ100について図3を用いて説明する。赤外線センサ100は、図3に示すように、上述した光学フィルタ1を備えている。また、赤外線センサ100は、赤外線検出素子110と、IC素子120と、基板130と、金属ケース150とを備えている。
次に、本実施形態に係る発光装置200について図4を用いて説明する。発光装置200は、図4に示すように、上述の光学フィルタ1を備えている。また、発光装置200は光学フィルタ1に赤外線を含む光を照射する光源210を備えている。光源210は、LED、キセノンランプ、レーザーダイオード及びこれらの組み合わせを含んでいてもよい。
次に、本実施形態に係る光学フィルタ1の製造方法について説明する。光学フィルタ1は、無機物質の粒子と波長選択吸収材料との混合物を、溶媒を含んだ状態で加圧して加熱することにより製造することができる。このような加圧加熱法を用いることにより、無機物質の一部が溶出して無機物質同士が互いに結合するため、波長選択吸収材料20が内部に分散した光学フィルタ1を形成することができる。
(実施例1)
まず、無機粒子として、水に対する溶解度が0.134g/100mLであり、平均粒子径が5μmのフッ化リチウムの粉末(富士フィルム和光純薬株式会社、試薬特級)を準備した。また、波長選択吸収材料として、メラミンの粉末(富士フィルム和光純薬株式会社、試薬特級)を準備した。次いで、フッ化リチウム粉末とメラミン粉末とを、質量比率が99:1(体積比率が98.3:1.7)となるように、メノウ乳鉢とメノウ乳棒を用い、アセトンを加えて混合することにより、混合粉末を得た。
波長選択吸収材料を添加しなかった以外は実施例1と同様に試験サンプルを作製した。すなわち、実施例1で用いたフッ化リチウム粉末を、実施例1と同様に加熱及び加圧した。
(直線透過率)
まず、上記のようにして得られた試験サンプルをFT-IR装置で透過法によって測定し、図5に示す赤外線透過スペクトルを得た。なお、赤外線透過スペクトルの直線透過率は、厚さ1mmにおける直線透過率となるように、ランベルト・ベールの法則に基づいて換算されている。
TGを実施することにより、メラミンの質量減少率を測定した。なお、サンプルはアルミニウム製の容器に7.1mg入れ、空気を50mL/分で流入させ、100℃から560℃まで10℃/分の加熱速度で測定した。測定により得られたTG曲線を図6に示す。
実施例1及び参考例1の試験サンプルの相対密度を測定した。具体的には、まず、試験サンプルの体積及び質量を測定し、試験サンプルの見掛け密度を算出した。次に、試験サンプルの見掛け密度を、マトリックスであるフッ化リチウムの真密度で除することにより試験サンプルの相対密度を算出した。
(実施例2)
まず、無機粒子として、水に対する溶解度が0.134g/100mLであり、平均粒子径が1μmのフッ化リチウムの粉末を準備した。また、波長選択吸収材料として、PVDFを準備した。次いで、フッ化リチウム粉末とPVDF粉末とを、質量比率が99:1(体積比率98.5:1.5)となるように、メノウ乳鉢とメノウ乳棒を用い、アセトンを加えて混合することにより、混合粉末を得た。
混合粉末におけるフッ化リチウム粉末とPVDF粉末との質量比率を98:2(体積比率97.1:2.9)とした以外は、実施例2と同様にして試験サンプルを作製した。なお、試験サンプルの厚さは1057μmであった。
混合粉末におけるフッ化リチウム粉末とPVDF粉末との質量比率を97:3(体積比率95.6:4.4)とした以外は、実施例2と同様にして試験サンプルを作製した。なお、試験サンプルの厚さは1017μmであった。
混合粉末におけるフッ化リチウム粉末とPVDF粉末との質量比率を96:4(体積比率94.2:5.8)とした以外は、実施例2と同様にして試験サンプルを作製した。なお、試験サンプルの厚さは1014μmであった。
混合粉末におけるフッ化リチウム粉末とPVDF粉末との質量比率を92:8(体積比率88.6:11.4)とした以外は、実施例2と同様にして試験サンプルを作製した。なお、試験サンプルの厚さは1064μmであった。
PVDF粉末に代え、PTFE粉末(株式会社喜多村 KTL-1N)を用いた以外は、実施例2と同様にして試験サンプルを作製した。具体的には、混合粉末におけるフッ化リチウム粉末とPTFE粉末との質量比率を99:1(体積比率98.4:1.6)とした。なお、試験サンプルの厚さは1147μmであった。
混合粉末におけるフッ化リチウム粉末とPVDF粉末との質量比率を100:0とした以外は、実施例2と同様にして試験サンプルを作製した。なお、試験サンプルの厚さは1064μmであった。
(直線透過率)
上記のようにして得られた試験サンプルをFT-IR装置で透過法によって測定し、図7~図10に示す赤外線透過スペクトルを得た。なお、赤外線透過スペクトルの直線透過率は、厚さ1mmにおける直線透過率となるように、ランベルト・ベールの法則に基づいて換算されている。
TGを実施することにより、PTFE及びPVDFの質量減少率を測定した。なお、サンプルはアルミニウム製の容器にPTFEを5.5mg又はPVDFを6.2mg入れ、空気を50mL/分で流入させ、30℃から600℃まで10℃/分の加熱速度で測定した。測定により得られたTG曲線を図12に示す。測定の結果、PTFEの質量減少率が10質量%となる温度は456℃であり、PVDFの質量減少率が10質量%となる温度は400℃であった。
実施例2~実施例7及び参考例2の試験サンプルの相対密度を上記と同様に測定した。その結果、いずれの試験サンプルの相対密度も90%以上であった。このことから、試験サンプルの気孔率は小さく、試験サンプルは緻密な構造となっていることが理解できる。
10 マトリックス
20 波長選択吸収材料
100 赤外線センサ
200 発光装置
Claims (12)
- 水に対する溶解度が0.4g/100g-H2O以下である無機物質によって構成されたマトリックスと、
前記マトリックス内に分散された波長選択吸収材料と、
を備える光学フィルタであって、
前記光学フィルタは0.8μm~20μmの対象波長帯域におけるいずれかの帯域の波長を有する光成分を吸収し、
空気中で100℃から10℃/分の速度で加熱した場合において、前記波長選択吸収材料の質量減少率が10質量%となる温度は900℃以下であり、
前記マトリックスの真密度に対する前記光学フィルタの見掛け密度は70%以上であり、
前記対象波長帯域において、前記光学フィルタの厚さ1mmあたりの直線透過率が30%以上である波長帯域幅は50nm以上である、光学フィルタ。 - 前記質量減少率が10質量%となる温度は600℃以下である、請求項1に記載の光学フィルタ。
- 前記質量減少率が10質量%となる温度は300℃以下である、請求項1又は2に記載の光学フィルタ。
- 前記マトリックスを構成する無機物質は、フッ化物、酸化物及び酸化水酸化物からなる群より選択される少なくとも1種を含む、請求項1から3のいずれか一項に記載の光学フィルタ。
- 3μm~10μmの対象波長帯域において、前記直線透過率が30%以上である波長帯域幅は300nm以上である、請求項1から4のいずれか一項に記載の光学フィルタ。
- 3μm~10μmの対象波長帯域において、前記直線透過率が1%以下である波長帯域幅は300nm以上である、請求項1から4のいずれか一項に記載の光学フィルタ。
- 3μm~10μmの対象波長帯域において、前記直線透過率が30%以上である波長帯域幅は300nm以上であり、前記直線透過率が1%以下である波長帯域幅は300nm以上である、請求項1から4のいずれか一項に記載の光学フィルタ。
- 前記無機物質はフッ化リチウムを含む、請求項1から7のいずれか一項に記載の光学フィルタ。
- 前記無機物質はフッ化物を含み、前記波長選択吸収材料はフッ素樹脂を含む、請求項1から8のいずれか一項に記載の光学フィルタ。
- 8μm~20μmの波長帯域全体において、前記直線透過率は10%以下である、請求項1から9のいずれか一項に記載の光学フィルタ。
- 請求項1から10のいずれか一項に記載の光学フィルタを備える、赤外線センサ。
- 請求項1から10のいずれか一項に記載の光学フィルタを備える、発光装置。
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JPS6373203A (ja) | 1986-09-17 | 1988-04-02 | Sumitomo Bakelite Co Ltd | 粒子分散型複合赤外線バンドパスフイルタ |
JP2004240289A (ja) * | 2003-02-07 | 2004-08-26 | Seiko Epson Corp | マスク形成方法ならびにこの方法を用いて製造されたカラーフィルタ |
JP2015196622A (ja) * | 2014-04-01 | 2015-11-09 | 住友金属鉱山株式会社 | 熱線遮蔽膜、熱線遮蔽透明基材、自動車および建造物 |
WO2020195183A1 (ja) * | 2019-03-26 | 2020-10-01 | パナソニックIpマネジメント株式会社 | 複合部材、並びにそれを用いた発熱装置、建築部材及び発光装置 |
JP2021025009A (ja) | 2019-08-08 | 2021-02-22 | 東亞合成株式会社 | 布地、皮革又は紙用接着剤、布地、皮革又は紙の接着方法、及び布地、皮革又は紙製品の製造方法 |
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JPS6373203A (ja) | 1986-09-17 | 1988-04-02 | Sumitomo Bakelite Co Ltd | 粒子分散型複合赤外線バンドパスフイルタ |
JP2004240289A (ja) * | 2003-02-07 | 2004-08-26 | Seiko Epson Corp | マスク形成方法ならびにこの方法を用いて製造されたカラーフィルタ |
JP2015196622A (ja) * | 2014-04-01 | 2015-11-09 | 住友金属鉱山株式会社 | 熱線遮蔽膜、熱線遮蔽透明基材、自動車および建造物 |
WO2020195183A1 (ja) * | 2019-03-26 | 2020-10-01 | パナソニックIpマネジメント株式会社 | 複合部材、並びにそれを用いた発熱装置、建築部材及び発光装置 |
JP2021025009A (ja) | 2019-08-08 | 2021-02-22 | 東亞合成株式会社 | 布地、皮革又は紙用接着剤、布地、皮革又は紙の接着方法、及び布地、皮革又は紙製品の製造方法 |
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