CN109809689B - Substrate for optical filter and optical filter - Google Patents
Substrate for optical filter and optical filter Download PDFInfo
- Publication number
- CN109809689B CN109809689B CN201811397056.XA CN201811397056A CN109809689B CN 109809689 B CN109809689 B CN 109809689B CN 201811397056 A CN201811397056 A CN 201811397056A CN 109809689 B CN109809689 B CN 109809689B
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- filter
- filter glass
- substrate
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- glass
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- 230000003287 optical effect Effects 0.000 title claims abstract description 106
- 239000000758 substrate Substances 0.000 title claims abstract description 73
- 239000011521 glass Substances 0.000 claims abstract description 232
- 230000005540 biological transmission Effects 0.000 claims abstract description 137
- 230000000903 blocking effect Effects 0.000 claims abstract description 71
- 238000001228 spectrum Methods 0.000 claims abstract description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 16
- 229910003069 TeO2 Inorganic materials 0.000 claims abstract description 15
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 10
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 9
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 9
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 9
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 9
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000004040 coloring Methods 0.000 claims description 15
- 238000002834 transmittance Methods 0.000 claims description 15
- 239000011669 selenium Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 12
- 229910052711 selenium Inorganic materials 0.000 claims description 12
- 229910052717 sulfur Inorganic materials 0.000 claims description 12
- 239000011701 zinc Substances 0.000 claims description 11
- 239000006104 solid solution Substances 0.000 claims description 9
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- 230000007704 transition Effects 0.000 claims description 8
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 7
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- 239000011593 sulfur Substances 0.000 claims description 6
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 5
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- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 7
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- 238000000576 coating method Methods 0.000 description 7
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- 239000011248 coating agent Substances 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 6
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- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 4
- 239000000395 magnesium oxide Substances 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 4
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical compound [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 4
- VASIZKWUTCETSD-UHFFFAOYSA-N manganese(II) oxide Inorganic materials [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 4
- 229910004613 CdTe Inorganic materials 0.000 description 3
- KOPBYBDAPCDYFK-UHFFFAOYSA-N Cs2O Inorganic materials [O-2].[Cs+].[Cs+] KOPBYBDAPCDYFK-UHFFFAOYSA-N 0.000 description 3
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- 230000002411 adverse Effects 0.000 description 3
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 3
- AKUNKIJLSDQFLS-UHFFFAOYSA-M dicesium;hydroxide Chemical compound [OH-].[Cs+].[Cs+] AKUNKIJLSDQFLS-UHFFFAOYSA-M 0.000 description 3
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- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
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- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
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- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 2
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- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
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- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 2
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- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 description 1
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- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- YEAUATLBSVJFOY-UHFFFAOYSA-N tetraantimony hexaoxide Chemical compound O1[Sb](O2)O[Sb]3O[Sb]1O[Sb]2O3 YEAUATLBSVJFOY-UHFFFAOYSA-N 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000000411 transmission spectrum Methods 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 229910003454 ytterbium oxide Inorganic materials 0.000 description 1
- 229940075624 ytterbium oxide Drugs 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
- XSMMCTCMFDWXIX-UHFFFAOYSA-N zinc silicate Chemical compound [Zn+2].[O-][Si]([O-])=O XSMMCTCMFDWXIX-UHFFFAOYSA-N 0.000 description 1
- 235000019352 zinc silicate Nutrition 0.000 description 1
- UQMZPFKLYHOJDL-UHFFFAOYSA-N zinc;cadmium(2+);disulfide Chemical compound [S-2].[S-2].[Zn+2].[Cd+2] UQMZPFKLYHOJDL-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/11—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
- C03C3/066—Glass compositions containing silica with less than 40% silica by weight containing boron containing zinc
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/078—Glass compositions containing silica with 40% to 90% silica, by weight containing an oxide of a divalent metal, e.g. an oxide of zinc
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/08—Compositions for glass with special properties for glass selectively absorbing radiation of specified wave lengths
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/10—Compositions for glass with special properties for infrared transmitting glass
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/04—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of organic materials, e.g. plastics
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Abstract
The present invention relates to an improved substrate for an optical filter and an optical filter. The substrate comprises a filter glass containing SiO2、ZnO、K2Chalcogenide of O and cadmium, the filter glass being based on oxide, TeO2The content is 0.1 to 3 wt%, and the CoO content is 1.0 to 7.0 wt%, preferably>1.0 to 7.0 wt%. The filter glass has a first blocking range in the visible region of the spectrum, a passband in the near infrared region of the spectrum, a first transmission edge, and an edge wavelength λ 'between 700nm and 840nm based on a filter glass thickness of 0.3 mm'i0.5。
Description
Technical Field
The invention relates to a substrate for an optical filter comprising a filter glass, an optical filter and the use thereof.
Background
Optical filters are known for their characteristic transmission properties. Such a filter has at least one blocking range (in german, "sperrbergeich") and one pass-band (in german, "Durchlassbereich"). The blocking range is the region with as low a transmission as possible, while the pass band (also called pass region) refers to the region of the spectrum with high transmission. If the transmittance rises from a low transmittance to a high transmittance in a narrow spectral range, it is called transmission edge (transmission edge). Filters with steep transmission edges are also referred to as steep edge filters. The second blocking range may adjoin the pass band.
The transmission edge is realized in the glass by absorption and in the interference filter by interference.
Optical (sharp-edge) filters are characterized by specific characteristics. For example, for the position of the transmission edge of such a filter, the so-called edge wavelength λ for internal transmission (german "reintensision") may be reportedi0.5. It corresponds to the internal spectral transmission τ between the blocking range and the pass band of a defined thicknessiValue τi＝50％(Ti50) Wavelength (see DIN 58131).
Optical steep edge filters typically include a substrate that may take the form of a filter glass. In addition, at least one coating for establishing the desired optical properties may be present.
Color filter glasses (also known as tinted glasses or volume filters) comprise a more or less colorless base glass into which a tinted component (chromophore) is incorporated that selectively absorbs a specific proportion or greater of the incident light spectrum, depending on the nature of the component incorporated, giving the glass a tinted appearance. In the case of these colored glasses, a distinction is made between ion-colored glasses and annealed glasses, differing in the coloring process and in the absorption characteristics.
In the case of ion-tinted glass, the desired spectral transmission curve has generally been achieved by curing of liquid glass. Depending on the nature of the colouring component used, which is generally a compound of an element from the transition group of the periodic table of the elements, and of the base glass, a specific spectral region is absorbed. The absorption properties of the colored glass are caused by the absorption bands of the colored ions and by the base glass itself, wherein the absorption bands have a greater or lesser width. The dense matrix of colored ions is not uniform due to the amorphous and irregular structure of the glass. This results in a less steep progression of the different excitation energies and transmission curve edges. "short-wave" transmission edge (the edge is located towards the short-wave region of the spectrum, i.e. a first rising edge, hereinafter referred to as "first transmission edge", having an edge wavelength λ'i0.5(ii) a See also fig. 1) cannot be adjusted to any steepness.
Annealed glasses (also known as "semiconductor-doped glasses" or "colloidal colored glassesGlass "or" steeply edged tinted glass ", in german" analafglas "or" steilkandenfarbgas ", has a base glass to which one or more semiconductor components (dopants) have been added as tinting components. The dopants used are generally semiconductor dopants, in particular cadmium chalcogenides (CdS, CdSe, CdTe, individually or in any combination) and/or zinc (ZnS, ZnSe, ZnTe, individually or in any combination). A particular feature of annealed glasses is that they are usually in the form of colorless or pale colored glasses after production (by the melting route or by sintering) and cooling. The subsequent heat treatment process (annealing) colors the glass. Due to heating (tempering) of the glass to (transition temperature (T)g) -70 ℃ and (T)g+200 ℃ C, preferably (T)g+150 ℃ C.), T is particularly preferredgA suitable temperature between +120 ℃ (e.g., tempering in the range of 530 ℃ to 730 ℃) for a period of several minutes to several weeks, phase separation occurs in the glass and nanocrystals form in one phase, so the absorption of the annealed glass can be attributed to this. Depending on the respective doping, for example, chalcogenide crystals (cadmium sulfide/zinc sulfide, cadmium selenide/zinc selenide, and/or cadmium telluride/zinc telluride, and also solid solutions, if possible) are formed. Thus, the first transmission edge of the colorless or pale glass rises to a steep rise, which is characteristic of annealed glass, meaning that the first transmission edge becomes steeper and shifts to a greater or lesser wavelength.
Depending on the composition of the base glass, the composition of the semiconductor doping and the control of the temperature/time program, nanocrystals of different chemical compositions and sizes can be produced, thereby changing the edge position of the filter glass. Due to the formation of the semiconductor crystal and its conductive properties (band structure, energy gap between valence and conduction bands), the annealed glass absorbs incident white light from the UV range up to the visible range and in some cases even higher wavelengths in an almost quantitative manner, while wavelengths beyond the first transmission edge (also called annealing edge) are quantitatively transmitted. As the absorption region (blocking range) and the transmission region (pass band) are delimited from one another by steep edges, the annealed glass achieves a particularly pure color and therefore has particularly good filter properties.
Because of the steep first transmission edge, the position of which can be reproducibly adjusted with high accuracy by means of composition, melting conditions and tempering conditions, the annealed glass can be used as an optical filter (referred to as a steep edge filter) and as a substrate for an optical filter.
The patent literature has described various glass components which are suitable in principle as annealed glasses. Typical annealed glasses based on cadmium chalcogenides are known from DE 2621741 a1 and DE 10141105C 1. JP 50-11924B describes a Li-containing2O glass and glass containing a high BaO content, these glasses containing CdS, Se, and Te.
The glass of JP 44-23821A requires not only CdS but also iron oxide.
The glass of SU 192373 contains not only CdO, Se, S and C, but also PbO and Cu2And O. However, in PbO, CuO or Cu2In the case of both O and chalcogenide, there is a significant undesirable discoloration in the glass.
US 5,059,561 describes a uv absorbing annealed glass for sunglasses which is substantially free of annealed colour after tempering and formation of microcrystals. By adding colouring components such as NiO, CuO, V2O5、Ce2O3、CoO、Nd2O3、Er2O3And/or Sm2O3And (4) coloring.
Cadmium-free annealed glasses based on aluminosilicate glasses are also known (for example, DE 4231794C2), in which the crystallites consist predominantly of TiO2And ZrO2And (4) forming. Adding a large amount of coloring oxide (such as Cr)2O3、MnO2、Fe2O3、CoO、NiO、CuO、V2O5、CeO2、TiO2、Pr2O3、Nd2O3、Er2O3) Color loci (colour foci) are formed. A disadvantage of such glasses is that they do provide a red color sufficient for signaling systems and lighting purposes, but in that<1mm, in particular<With a low glass thickness of 0.5mm, no sharp edges and a tight barrier in the barrier range are provided.
EP 0536572A 1, EP 0496943A 1 describe colored opaque glass ceramics which contain small proportions of colored oxides (e.g. Cr2O3、NiO、Co3O4、V2O5) For coloring. Such glass-ceramics cannot be used as optical filters.
For some applications it may be advantageous to use optical filters with high transmission, in particular only for a defined part of the spectrum, for example the end of the red region of the visible spectrum and wavelengths in the near infrared region of the spectrum (NIR region) to, for example, 1000 nm. Typically, the NIR region of the spectrum comprises wavelengths of 780nm to 3000 nm.
Certain optical applications require that when the filter is used, for example, in conjunction with a sensor, the filter has a particularly high transmission in certain regions of the spectrum and as low a transmission as possible in other regions, and therefore should be transparent only to light of a particular wavelength range. For example, for applications in the red region and NIR of the spectrum, using an LED emitting radiation in the wavelength range of about 700nm to about 980nm, the wavelength range will be detected by the sensor. In order to improve the measurement results of the sensor, an optical filter is inserted in front of the sensor, which optical filter is highly transparent to the desired wavelengths and has as low a transparency as possible to other regions of the spectrum. Such optical filters having a pass band on either side defined by a blocking range are referred to as bandpass filters.
The band-pass filters used to date are generally multilayer systems or interference filters having a (colorless) substrate and a plurality of filter layers applied, the filter effect of which is based on reflection. Since light is not absorbed in these layers, multiple reflections often occur in the corresponding lens system, which results in "ghosts" (in german, "gersterderlder"). By the design of the filter layers, a plurality of filter curves can be achieved, one characteristic of which is that they have steep edges on either side between the pass band and the blocking range. A disadvantage of interference filters is that they have a strong dependence on the angle of incidence of the incident light and a wide and high blocking can be achieved only by a very large number of layers. Therefore, multilayer systems with the required filter function with steep edges are very expensive.
In the context of component miniaturization, it is also desirable in the case of filters to achieve the desired filter performance with a smaller overall filter thickness. Even tinted glasses that achieve sufficient blocking in the blocking range with a thickness of 1mm to 3mm (the thicknesses customary to date) exhibit an undesirable residual transmission, i.e. a certain transmission, in the blocking range with a lower thickness (thickness <1 mm). In the case of low substrate thicknesses or filter thicknesses of <0.3mm, the transmission in the blocking range is generally still 20% even in the case of annealed glasses, which means that additional measures (for example in the form of additionally applied filter layers, for example interference filter layers) are required in order to achieve a sufficient blocking of the transmission in the blocking range.
Disclosure of Invention
Starting from this problem, it is an object of the present invention to provide a substrate based on a filter glass for optical filters having a passband in the NIR region, wherein the substrate has steep edge filtering properties, has a first transmission edge between 700nm and 840nm, and has an improved blocking by absorption in the blocking range at low substrate thicknesses (<1 mm).
This object is achieved by a substrate for an optical filter according to claim 1 and an optical filter comprising a substrate according to claim 10.
According to the present invention, a substrate for an optical filter includes a substrate containing SiO2、ZnO、K2Filter glass of chalcogenide of O and cadmium based on oxide, TeO2The content is 0.1 to 3 wt%, the CoO content is 1.0 to 7.0 wt%, preferably>1.0 to 7.0 wt%. The filter glass has a first blocking range in the visible region of the spectrum, a passband in the near infrared region of the spectrum, and an edge wavelength λ 'between 700nm and 840nm based on a filter glass thickness of 0.3 mm'i0.5Having a first transmissive edge.
For the first transmissive edge, edge wavelength λ'i0.5Refers to the internal spectral transmission τ between the first blocking range and the pass band at a thickness of 0.3mmiValue τi0.5 (corresponding to 50%) (or Ti50I value).
It is basically known that the edge wavelength λ 'of the transmission edge'i0.5Depending on the thickness of the glass. The numbers (figures) given below relate to a filter glass thickness of 0.3 mm. The skilled person will be able to deduce the position of the transmission edge for other filter glass thicknesses.
Substrates for optical filters may include a filter glass and optionally additional components applied thereto (e.g., adhesion promoter layers, layers for improving chemical stability, absorbing layers). In an advantageous embodiment, the filter glass forms a substrate for an optical filter, on which one or two or more coatings (applied to one or both sides of the filter glass) are applied to produce the optical filter.
In the context of the present invention, the filter glass comprises a base glass based on SiO as network former2ZnO as a network-forming body and a network-modifying body, and K as a network-modifying body2And O. As a dopant for coloring, the filter glass contains a semiconductor dopant substance forming a chalcogenide of cadmium (CdS, CdSe, CdTe, and a solid solution having a chalcogenide of zinc such as (Zn, Cd) (S, Se, Te)). Thus, the filter glass is annealed glass. In the filter glass, the colored glass component is present in particular in reduced form. However, all glass components are hereinafter expressed in weight% of oxides.
TeO2The effect of the content in the cadmium-containing chalcogenide filter glass is that by means of a corresponding heat treatment it is possible to establish a filter glass having a boundary wavelength λ 'between 700nm and 840 nm'i0.5The first transmissive edge of (a). One effect of the high CoO content in the glass is additional absorption in the blocking range outside the first transmission edge. At low filter glass thicknesses this results in lower residual transmission in the blocking range, i.e. higher optical density, higher blocking.
Edge wavelength λ 'of the first transmissive edge, by design'i0.5I.e. the position of the first transmission edge, may be 700nm, preferably 720nm, further preferably 740nm, advantageously 760nm, further advantageously 780nm, yet advantageously 800nm, further advantageously 820nm, advantageously 840nm at a filter glass thickness of 0.3 mm. Advantageously, the edge wavelength λ 'of the first transmission edge is based on a filter glass thickness of 0.3 mm'i0.5May be between 740nm and 820 nm.
With regard to the filter properties of the filter glass or of the optical filter, it is advantageous if, when the filter glass has a thickness of 0.3mm, the first transmission edge has an internal transmission of 15%, preferably 10%, up to an internal transmission of 90% or more in the region of a width of 150nm or less, preferably 130nm or less, preferably 120nm or less, preferably 110nm or less, particularly preferably 100nm or less, and also preferably 80nm or less. This results in a particularly narrow transition region between the blocking range and the pass band, which is advantageous for the subsequent use of the optical filter. Therefore, the filter glass has a steep first transmission edge.
Advantageously, the thickness of the filter glass can be <1mm, preferably < 0.75mm, preferably < 0.5mm, also preferably <0.3mm, particularly preferably < 0.25, further preferably < 0.2 mm. The filter glass is thus an annealed filter glass in the form of a thin glass. The low thickness makes it particularly suitable for producing miniaturized filters for optical and other applications.
In an advantageous embodiment of the invention, the filter glass has an internal transmission or spectral internal transmission of less than 15%, preferably 10%, more preferably 5%, particularly preferably 1%, in the wavelength range between 400nm and 680nm, i.e. in a section of the first blocking range, based on a thickness of 0.3 mm. The low residual transmission in the visible region makes it possible to significantly reduce or even completely dispense with the additional costs hitherto required for blocking the residual transmission (for example, the application of additional filter layers, for example interference filter layers). In an advantageous variant of the filter glass, there is an internal transmission of less than 15%, preferably less than or equal to 10%, more preferably less than or equal to 5%, particularly preferably less than or equal to 1%, in the wavelength range between 300nm and 700nm, based on a filter glass thickness of 0.3 mm.
In an advantageous development of the invention, the high CoO content in the filter glass achieves the effect that the filter glass has a second blocking range in the near infrared region (NIR region), with an IR edge wavelength λ ″, based on a filter glass thickness of 0.3mm "i0.5Is between 950nm and 1300 nm. Thus, especially TeO2And a high CoO content cadmium-containing chalcogenide containing annealed glass, wherein the passband (depending on the location of the first transmission edge) may also include portions of the red spectral region of visible light. The second blocking range adjacent to the pass band in the direction of the infrared region of the spectrum can be significantly reduced or, depending on the respective application, even completely eliminate the costs hitherto required for reducing transmission in the NIR region (for example, the application of additional filter layers, for example interference filter layers).
For the second transmission edge, the edge wavelength λ "i0.5Representing the internal spectral transmission τ between the pass band and the second blocking range at a thickness of 0.3mmiValue τi0.5 (corresponding to 50%) (or Ti50Value of II).
According to various embodiments, the edge wavelength λ of the second transmission edge "i0.5I.e. the position of the second transmission edge, may be 950nm, preferably 975nm, further preferably 1000nm, advantageously 1025nm, further advantageously 1050nm, further advantageously 1075nm, further advantageously 1100nm, advantageously 1125nm, advantageously 1150nm, advantageously 1175nm, advantageously 1200nm, advantageously 1225nm, advantageously 1250nm, advantageously 1275nm, advantageously 1300nm at a filter glass thickness of 0.3 mm.
The pass band of the filter glass or optical filter should have as high an internal transmission (tau) as possiblei). In an advantageous development of the invention, the internal transmission in the section within the pass band, i.e. for the wavelength range within the pass band, is at least 85%, preferably at least 90%, more preferably at least 91%, even more preferably at least 95%, based on a filter glass thickness of 0.3mm. When the wavelength range having the above-specified high internal transmittance is within>100nm, preferably>130nm, preferably>It is more advantageous when the extension is in the range of 150 nm. Preferably, the pass band with the desired high internal transmission can be in the wavelength range between 720nm and 1100nm, preferably between 750nm and 1000nm, particularly preferably between 780nm and 950nm for the specific application.
In an advantageous embodiment of the invention, the filter glass of the substrate of the invention comprises the following composition (in% by weight based on the oxides):
the glass component of the filter glass is explained in detail below. These components are described in the conventional manner in the form of oxides. However, this is not a statement as to the form of the raw materials of the respective components used for glass production and the form of the respective components actually present in the glass (for example selenium may be used as SeO2Can also be used as Se2-Present in the glass).
Silicon dioxide (SiO)2) Is used as a network former and constitutes 39 to 50% by weight, preferably 40 to 46% by weight, of the main constituent of the glass. The level should not be below the lower limit of 39% by weight, since otherwise the chemical stability of the glass would be reduced. Another advantageous lower limit may be 40 wt% or 41 wt%. SiO 22The upper limit of the content should be not more than 50% by weight. This upper limit should not be exceeded because otherwise the melting temperature would rise too significantly and the extent to which the volatile colored Cd (S, Se, Te) compounds evaporate from the glass would increase. An advantageous embodiment of the glass comprises at most 46% by weight, preferably at most 45% by weight, of SiO2. In a preferred embodiment, the glass of the invention comprises less than 45% by weight of SiO2。
Another important component is zinc oxide (ZnO). The ZnO effects crystallization of the dopant in a uniformly distributed region of the glass. Thus, uniform crystallite growth of the semiconductor dopant occurs in the subsequent tempering of the glass, forming crystallites with a very narrow size distribution. This results in a very pure "color" and a steep first transmission edge of the filter glass according to the invention. A high Zn content is also advantageous in glass production, since a solid solution of cadmium and zinc is thus formed together with the chalcogenide. Zinc helps to keep the chalcogenide in the melt due to its high affinity for sulfur. As a result, the loss of sulfur during glass melting is reduced due to the reduction of burn-off. The component is present in the glass at 20 wt.% to 32 wt.%. An advantageous range can also be 22 to 31% by weight, preferably 23 to 31% by weight. The upper limit of 32 wt.% should not be exceeded because glasses with high ZnO content have a tendency to form droplet-like precipitate zones. Advantageously, the upper limit may therefore also be 31% by weight or 30% by weight. For ZnO, the level should not be below the lower limit of 20 wt% because otherwise the desired effect described above cannot be achieved. A further advantageous lower limit may be 22% by weight, advantageously 23% by weight, preferably 25% by weight. For some advantageous variants, 27 wt% may be an advantageous lower limit.
Since "zinc silicate glass" has a high tendency to separate, the filter glass advantageously contains potassium oxide (K)2O) as a network modifier in a proportion of 15 to 35% by weight. An advantageous range can also be from 18% to 30% by weight, preferably from 18% to 25% by weight. In order to prevent microprecipitations of the ZnO-rich regions, in order to increase the chalcogenide solubility in the filter glass, in order to reduce the processing temperature of the glass and in order to be able to match the coefficient of thermal expansion, the filter glass advantageously contains at least 15% by weight of K2And O. A further advantageous lower limit may be 18% by weight, preferably 20% by weight. The upper limit of 35 wt.% should not be exceeded, since otherwise the chemical stability becomes too poor and the coefficient of thermal expansion is too high. Thus, advantageously, K2The upper limit of O may be 30% by weight, preferably 27% by weight, preferably 25% by weight.
The potassium oxide may consist to a relatively small extent of sodium oxide (Na) in the base glass2O) instead. Na (Na)2O may advantageously be present in the glass in an amount of 0 to 5% by weight. In the presence of TeO2Annealing ofIn glass and annealed glass with high ZnO content, Na2O is not as good as K2O is suitable for establishing the desired filtering properties. There is a risk of undesirable crystallization of the Na-Zn silicate. In addition, higher Na2The O content reduces the chemical stability. Therefore, the upper limit of 5 wt% should not be exceeded. A further advantageous upper limit may be 4% by weight, preferably 3% by weight, preferably 2% by weight, and also preferably 1% by weight. When Na is present2When O is present in the glass, 0.01 wt.% may be a favorable lower limit. Na (Na)2Preferably, O is not intentionally added as a component of the batch (batch), but rather enters the glass through a source for another glass component, such as a cationic component as a selenium source. In this case, Na2O is not a raw material impurity but a concomitant raw material, but is not a mandatory glass component. However, when, for example, a different selenium source is used, there is no added Na other than the conventional impurities2Variants of O are also possible.
In a preferred variant of the invention, Na of the filter glass2O/K2O ratio (% by weight based on oxide)<1, advantageously<0.5, also advantageously<0.3, preferably<0.2, preferably<0.1, particularly preferably<0.08, further preferred<0.05。Na2O/K2The O ratio is favorable for establishing the thermal expansion coefficient.
In some variants, the filter glass (preferably by replacing K)2O) may contain not more than 5% by weight of Rb2O and/or not more than 5 wt.% Cs2O and/or less than 1 wt.% Li2And O. However, this is less preferred with respect to material costs. Advantageous variants may be Rb-free2O and/or Cs2O and/or Li2And O. If at least one of these components is present in the filter glass, 0.01% by weight can be an advantageous lower limit in each case. In one variant, no more than 2% by weight, advantageously no more than 1% by weight, of Rb is present2O, and/or not more than 2% by weight, advantageously not more than 1% by weight of Cs2O。Li2An advantageous upper limit for O may be<1% by weight.
In order to improve the meltability of the filter glass,may contain the proportion>0% to 4% by weight of boron oxide (B)2O3). A favorable lower limit may be 1 wt%. However, have<1% by weight of B2O3Or does not contain B2O3Variations of (2) are also possible. When the filter glass contains not more than 4% by weight, preferably less than 4% by weight (e.g. 3% by weight or 2% by weight) of B2O3It may be advantageous. B is2O3Too high a content may deteriorate the chemical stability of the glass.
In the context of the present invention, the filter glass may preferably be free of added alkaline earth oxides RO (i.e. free of MgO, CaO, SrO and BaO). Some variants may contain one or more alkaline earth metal oxides (calcium oxide (CaO), magnesium oxide (MgO), strontium oxide (SrO), barium oxide (BaO)) to adjust viscosity and coefficient of thermal expansion, and improve fusibility and processability. Like the alkali metal oxides, they are network modifiers. In the context of the present invention, its content (i.e. the sum of RO (R ═ Mg, Ca, Sr, Ba)) should not exceed a value of at most 10% by weight, preferably at most 8% by weight, since the softening temperature would increase too significantly and the solubility of the chalcogenide would decrease too significantly. The lower limit of the sum of RO may be 0.01 wt%.
Some variants may have MgO and/or CaO and/or BaO and/or SrO present, for example each in a proportion of at least 0.01% by weight. The upper limit of each component is 7% by weight.
Other components which may optionally be present in the base glass:
fluorine (F) may optionally be present in the glass. The lower limit, if present, may be 0.01 wt%. The presence of F lowers the melting temperature, thereby reducing the evaporation of volatile glass components. The upper limit of 3% by weight, advantageously 2% by weight, preferably 1% by weight, should not be exceeded, since the evaporation of F can lead to streaks. Moreover, high fluorine concentrations may cause the melting vessel to dissolve. Thus, a particularly advantageous variant does not contain F.
The glass may further contain up to 3% by weight of TiO2Up to 3% by weight of Al2O3And/or up to 10 wt.% of P2O5. A suitable lower limit for each of the components mentioned may be 0.01% by weight. TiO 22The blocking of UV can be improved, but also has an adverse effect as a nucleating agent for undesired crystal phases and can lead to a poor coloring effect, so that the upper limit of 3 wt.% should not be exceeded. An advantageous variant may be TiO-free2. Al may be used2O3To improve acid resistance and to lower the melting temperature. However, it should not exceed 3 wt% of Al2O3Upper limit, as the base glass may thus become more crystallization sensitive. In an advantageous embodiment, no more than 2% by weight, preferably no more than 1% by weight, preferably no more than 0.5% by weight, particularly preferably no more than 0.1% by weight, of Al can be present in the filter glass2O3. Variants may be free of added Al2O3。P2O5The meltability/sinterability is improved. However, since it has an adverse effect on the coefficient of thermal expansion and chemical stability, it is preferred to use only up to 5% by weight, particularly preferably only up to 3% by weight. Particularly preferred variants do not contain P2O5。
For example, refractory oxides, i.e., oxides of zirconium, niobium, tantalum, and lanthanum, may be used to improve chemical stability and/or affect the coefficient of thermal expansion, TgAnd operating temperature (V)A). Due to their poor meltability/sinterability, their tendency to crystallize and undesirable coloring effects in some cases, and their high cost, they are added only up to 5% by weight, preferably up to 3% by weight. A suitable lower limit for each of the components mentioned may be 0.01% by weight. Advantageous variants are free of zirconium oxide and/or niobium oxide and/or tantalum oxide and/or lanthanum oxide.
The dopant component for coloration present in the filter glass according to the invention is preferably CdO, SeO2、TeO2And SO3. The crystal or solid solution is formed of cadmium (Cd) and zinc (Zn) as cation components and sulfur (S), selenium (Se), and tellurium (Te) as anion components. The crystals formed can be described as (Cd, Zn) (S, Se, Te), wherein the components separated by commas within a set of brackets can be replaced by one another within a wide range.
Cadmium oxide (CdO) is advantageously present in the filter glass in an amount of 0.1 to 3% by weight. A preferred range may be 0.2 to 2 wt%, preferably 0.3 to 1 wt%. The level should not fall below the lower limit of 0.1 wt% otherwise too little CdO is available during the tinting process. An advantageous lower limit for CdO may also be 0.2 wt.%, preferably 0.3 wt.%, more preferably 0.4 wt.%. The upper limit of 3 wt.% should not be exceeded, since the CdO content during processing and in the product should be kept relatively low due to its toxicity. It can also be advantageous when no more than 2.5% by weight, preferably no more than 2% by weight, more preferably no more than 1.5% by weight, and particularly preferably no more than 1% by weight, of CdO is present in the filter glass.
Sulfur trioxide (SO)3) Advantageously present in the filter glass in an amount of from 0.05 to 1% by weight. A preferred range may be 0.07 to 0.7 wt%, preferably 0.1 to 0.5 wt%. The level should not be below the lower limit of 0.05 wt.%, otherwise too little SO3Can be used in coloring process. In addition, the sulfur or added sulfur-containing feedstock components act as a reducing agent in the melt. Combustion of S produces volatile SO2Which at the same time acts as a clarifying agent (fining agent) by bubble formation. SO (SO)3An advantageous lower limit of (b) may also be 0.07% by weight, preferably 0.1% by weight. The upper limit of 1 wt.% should not be exceeded because of K2SO4Or Na2SO4The destructive phase (sulfate bile) may precipitate out of the glass. When SO is present in the filter glass in an amount of not more than 0.7% by weight, preferably not more than 0.5% by weight, more preferably not more than 0.4% by weight, and particularly preferably not more than 0.3% by weight3It may also be advantageous.
Selenium dioxide (SeO)2) Advantageously present in the filter glass in an amount of from 0.1 to 1.5% by weight. A preferred range may be 0.2 to 1 wt%, preferably 0.3 to 0.7 wt%. The level should not be below the lower limit of 0.1 wt.%, otherwise too little SeO2Can be used in coloring process. In chalcogenide crystals, CdS and CdSe form a solid solution due to the corresponding lattice structure. SeO2An advantageous lower limit of (b) may also be 0.2% by weight, preferably 0.25% by weight, more preferably 0.3% by weight. The upper limit of 1.5 wt.% should not be exceeded because of SeO2Readily evaporate at higher temperatures and sublime again at other colder sites. SeO2Is also one of the toxic and expensive components, and therefore its content should be kept relatively low. When SeO is present in the filter glass in an amount of not more than 1% by weight, preferably not more than 0.7% by weight, preferably not more than 0.5% by weight2It may also be advantageous.
Tellurium dioxide (TeO)2) It is important for the position of the first transmission edge to be achieved at the end of the visible spectrum or at the beginning of the NIR region, which is desired in the context of the present invention. Thus, TeO2The content in the filter glass is 0.1 to 3 wt%. A preferred range may be 0.15 to 2 wt%, preferably 0.2 to 1 wt%. The level should not fall below the lower limit of 0.1 wt.%, otherwise too little TeO2Can be used for the required coloring process. In chalcogenide crystals, CdS and CdSe form a solid solution due to their similar crystal lattices. CdTe is incorporated into these solid solutions. TeO2An advantageous lower limit of (b) may also be 0.15% by weight, preferably 0.2% by weight. The upper limit of 3% by weight should not be exceeded because of the higher content of TeO2Without causing the position of the first transmission edge to shift to even higher wavelengths. Furthermore, similar to SeO2，TeO2Is toxic and relatively expensive, so it should not be used in higher concentrations. When TeO is present in the filter glass in an amount of not more than 2.5% by weight, preferably not more than 2% by weight, preferably not more than 1.5% by weight, and preferably also not more than 1% by weight2It may also be advantageous. Advantageous variants may contain not more than 0.7% by weight or not more than 0.5% by weight.
In addition to the cadmium chalcogenide, the filter glass of the substrate or filter according to the invention contains 1 to 7% by weight, preferably >1 to 7% by weight, of cobalt oxide (CoO).
The filter properties of the filter glass according to the invention are based firstly on the typical color formation mechanism of annealed glass and secondly on the typical ion-tinted glassA type color formation mechanism. Surprisingly, it has been found in the context of the present invention that when the filter glass is used as the thickness<When a 1mm thin substrate is used as an optical filter, it contains TeO2Such high CoO content in the annealed glass of (1) is feasible and advantageous. Due to the absorption band of CoO in the heat radiation region, it has been acknowledged so far that the absorption band is in the TeO-containing range2Such a high CoO content in the annealed glass (which is intended to be suitable for filters and thus has high requirements on optical properties and homogeneity) is not possible. In order to increase the blocking in the visible region of the spectrum significantly and to produce a second blocking range in the NIR region, CoO should be present in the filter glass in at least 1% by weight, preferably more than 1% by weight. A further advantageous lower limit may be 1.25 wt.%, preferably 1.5 wt.%, more preferably 1.7 wt.%, still preferably 2 wt.%. The upper limit should not be exceeded by 7 wt.%, otherwise the high internal transmission required in the pass band would deteriorate. In an advantageous variant, it is also possible for CoO to be present in an amount of not more than 6% by weight, preferably not more than 5% by weight.
Optionally, manganese (II) oxide (MnO) may be present in the filter glass as a colouring component in a proportion of 0 to 5 wt.%. It may be advantageous to use MnO in the case of thin filter glass in order to support the absorption effect of CoO. When MnO is present in the glass, an advantageous lower limit may be 0.05 wt.%, preferably 0.1 wt.%, more preferably 0.5 wt.%, still more preferably 1 wt.%. An advantageous upper limit may also be 4% by weight, 3% by weight or 2% by weight.
In one embodiment, the glass consists of the component SiO2、ZnO、K2O、B2O3、CdO、SO3、SeO2、TeO2And CoO to the extent of 95 wt%, preferably 98 wt%, more preferably 99 wt%.
The glasses according to the invention are preferably free, as filter glasses, of oxides of other colouring components (e.g. Cu, Fe, Cr and/or Ni) and/or of optically active components (e.g. laser-active components), for example of Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er and/or Tm. Furthermore, the glass preferably does not contain components harmful to health, such as oxides of Hg, Pb and TI. The glass according to the invention is further preferably free of radioactive constituents, such as oxides of Th and U.
The glass according to the invention preferably does not contain any bismuth oxide, rare earth metal oxides such as niobium oxide, yttrium oxide, ytterbium oxide, gadolinium oxide and tungsten oxide and/or zirconium oxide, with the exception that, as mentioned above, lanthanum oxide La may be present2O3. Niobium oxide is sparingly soluble in the melt. Further, niobium is a multivalent ion that participates in the redox balance in the melt. Zirconia and/or ytterbia increase the risk of glass crystallization. Yttria can degrade the weathering stability of the glass. In addition, the glass preferably does not contain platinum (Pt). Platinum and other metals from the Pt group (Ru, Os, Rh, Ir, Pd) have a destructive effect on optical performance. This can lead to scattering effects and color changes. Therefore, less than 3ppm, preferably less than 2ppm, preferably less than 1ppm should be present in the glass.
In one embodiment of the invention, the glass according to the invention is also preferably free of other components not mentioned in the claims or in the description; in other words, in such embodiments, the glass consists essentially of the above-described components, with the possible exception that the individual components mentioned are not preferred or less preferred. The expression "substantially … consists of (contained) means herein that the other components are present in the form of no more than impurities, but are not intentionally added to the glass composition as separate components.
If the glass is described as containing no component or containing no component, this means that the component may be present in the glass at most as an impurity. Meaning that it is not added in significant amounts or as a glass component, if any. According to the present invention, an insignificant amount is an amount of less than 100ppm, preferably less than 50ppm, most preferably less than 10 ppm. However, these limitations do not apply to Na2O, which may be present in the glass as a accompanying raw material in a relatively high proportion, but is advantageously less than 2% by weight, preferably less than 1% by weight.
In the case of the glass according to the invention, fining is preferably effected primarily by physical fining, which means meltingGlass at fining temperature has sufficient fluidity to allow bubbles (e.g. volatile SO)2) It may rise.
The glass according to the invention may include small amounts of conventional fining agents. Preferably, the total amount of added fining agent is at most 1.0 wt%, more preferably at most 0.5 wt%. Sb2O3And As2O3May be present in the glass but does not exhibit any fining effect since the glass melts under reducing conditions. In addition to chalcogenides, the glasses according to the invention may comprise as fining agent (in% by weight) at least one of the following components:
Sb2O30-1 and/or
As2O30-1 and/or
Halide (Br, Cl, F) 0-1.
The filter glass for a substrate according to the present invention may be melted and refined from raw materials by a melting method conventionally used for annealing glass, i.e., under reducing conditions at a temperature of about 1100 c to 1550 c, preferably 1220 c to 1360 c. During cooling, the glass is preferably formed into the desired shape. To form the coloration (i.e. for annealing), the blank thus obtained is heated again (tempered) within a defined temperature/time program.
For this purpose, the filter glass is described in [ T ]g-70℃]To [ T ]g+150℃]Is subjected to a further heat treatment, for example tempering in the range of 530 ℃ to 730 ℃ for a period of hours to weeks. The nanocrystallites consisting of Cd and Zn with S, Se, Te are formed here by colour components dissolved in the glass, the band gap between the valence band and the conduction band of which is determined firstly by the composition of the crystallites and secondly by the size of the crystallites. Which in turn depends on the annealing temperature and the annealing time. The higher the temperature and/or the longer the annealing time, the larger the crystallites will be, the smaller the band gap will be, and the longer the inherent color wavelength of the glass will be. The band gap approaches the limit of a macroscopic crystal of the same composition in an asymptotic manner. After the annealing process is completed, the typical transmission characteristics of glass, i.e., the transmission characteristics of a steep edge filter, are formed. Characterised by a blocking range (absorption) at short wavelengthsA pass-band region) and a very abrupt transition to almost complete transmission at slightly higher wavelengths, referred to as the pass-band or pass-through region. Preferably less than 150nm between the blocking range and the pass band.
It is also possible to produce the substrate according to the invention by known sintering routes. For this purpose, for example, a green body obtained from a suspension containing the necessary glass components is dried after solidification and sintered and/or melted at a temperature between 600 ℃ and 1200 ℃. Sintering processes based on powder methods are also possible. An annealing treatment is carried out after the production of the glass blank to form cadmium-chalcogenide crystals in the temperature/time program required in each case.
The invention also provides an optical filter comprising a substrate according to the invention comprising a filter glass having a first steep transmission edge (i.e. a steep edge filter, preferably a bandpass filter) with a defined passband, and at least one optical layer for adjusting the spectral transmittance of the optical filter. The at least one optical layer may increase the blocking within a desired blocking range and/or increase the steepness of the transition between the blocking range and the pass band and/or increase the transmission in the pass band and/or create a narrow band pass filter in the pass band. The narrow band pass filter in the context of the present invention has a spacing with a high spectral transmission defined by steep edges, wherein the spacing width (FWHM, see also DIN ISO 9211-2) is not more than 150nm, preferably not more than 80nm, preferably not more than 25nm, more preferably not more than 15 nm.
The substrate is preferably a substantially uniform, flat and thin element, which means that it has two opposite sides, in each case the substrate surface of the substrate being large relative to the thickness of the substrate.
The substrate or filter glass of the optical filter may be coated on one or both sides. In the case of one-sided coating, only one substrate surface has an optical layer. In the case of two-sided coating, each of the two opposing substrate surfaces has an optical layer. It is of course also possible to provide two or more optical layers per substrate surface.
In a first advantageous embodiment, the optical layer is an interference layer, preferably a multilayer interference system. In another advantageous embodiment, the optical layer is a coating comprising an absorbing component. The optical layer has the function of increasing the spectral transmittance in one or more defined sections of the spectrum (anti-reflection effect) and/or increasing the blocking in one or more regions. It may also be used to increase the steepness of the transition between blocking range and pass band and/or to create a narrow band pass filter in the pass band. At the same time, at least one optical layer may serve as a protective layer to increase the stability of the filter glass to environmental influences. Undesired residual transmission in the blocking range of the filter glass (in particular in the second blocking range) can also be blocked by a suitably configured optical layer; in this case, the at least one optical layer may also have an absorbing effect.
The at least one optical layer can preferably be designed as a multilayer interference system in order to contribute to the filter effect of the filter glass and to fulfill the functions described above. However, interference filters have angle-dependent edges: in other words, the optical filter has a "color" shift that depends on the angle of incidence.
Advantageously, the thickness of the optical filter can be <1mm, preferably ≦ 0.75mm, more preferably ≦ 0.5mm, still more preferably ≦ 0.3mm, particularly preferably ≦ 0.25, further preferably ≦ 0.2 mm.
The optical properties of an optical filter are determined by the properties of the optical layer and the properties of the substrate or filter glass.
As described above, the filter glass according to the invention in an optical filter has a passband in the red and/or NIR region of the spectrum, with a steep first transmission edge. In a section within the pass band, the internal transmission of the filter glass with a thickness of 0.3mm preferably amounts to at least 85%, preferably 90%. This region, i.e. the region with a particularly high internal transmission, is advantageously in the wavelength range from 750nm to 950 nm.
The filter glass according to the invention has a steep first transmission edge due to its composition and heat treatment, which is advantageous for the production of the optical filter according to the invention, since the steep first transmission edge of the optical filter towards the short-wave region of the spectrum can already be provided by the filter glass itself and does not need to be produced by complex optical layers (e.g. complex angle-dependent multilayer systems). Of course, the first transmission edge of the optical filter may still be modified by applying the multilayer system and/or coating. The first steep transmission edge of the filter glass has the following advantages: the short-wave edge of the optical filter is no longer significantly influenced by the applied layer system.
It is also known that many optical bandpass filters formed by multilayer interference systems have the disadvantage that, in addition to the desired and specially designed pass band, they can also have other regions of increased transmission in the visible region of the spectrum (called sub-maxima). Since the optical filter according to the invention comprises a filter glass according to the invention which has a blocking range in the visible region of the spectrum, these sub-maxima do not adversely affect the transmission properties of the optical filter. Thus, for example, the design of a multilayer interference system can be simplified.
By means of one or more optical layers applied to the substrate according to the invention, the passband defined by the filter glass can thus be varied, e.g. narrowed specifically, for a specific application of the optical filter. The at least one optical layer is used to change the spectrum of the filter glass. The filtering effect of the glass is therefore assisted by at least one optical layer, in particular in the form of an interference layer system.
In an advantageous embodiment of the substrate for optical filters according to the invention, the filter glass has a second blocking range in the near infrared region (NIR region) (see above). Therefore, this filter glass selectively transmits only a spectrum of a narrow wavelength range from a red region to a near infrared region. The second transmission edge of the filter glass towards the IR region may also be tuned by one or more optical layers to tune the spectral transmittance of the optical filter.
By combining the filter glass substrate according to the invention with at least one suitable optical layer, it is thus possible to optimally adapt the optical filter according to the invention to the respective requirements arising from the respective field of use. By using the substrate of the invention with the described filter properties and an optical layer or optical layers, a plurality of individually adapted optical filters for various applications can be produced in various ways.
The optical filter may preferably be a filter with band-pass properties having a first blocking range in the visible region of the spectrum and a second blocking range in the NIR region of the spectrum. Between the blocking ranges where the optical filter has a very effective blocking, there is a pass-band, the width and exact position of which depends on the individual use at a later time. The pass band of the optical filter is in the wavelength range between 700nm and 1100 nm.
In a preferred embodiment, the filter glass substrate according to the invention is provided as a thin plate-like element and the interference filter system is present on one or both (advantageously polished) sides, so that at least one of the following bandpass properties of the filter glass is improved: increasing the blocking in the desired blocking range and/or increasing the steepness of the transition from the blocking range to the pass band and/or increasing the transmission in the desired pass band and/or creating a narrow band pass filter in the pass band. By means of the inventive combination of the filter glass according to the invention and the at least one optical layer, it is possible in particular to produce narrow-band bandpass filters which are not possible in the form of pure filter glasses and which can be implemented as pure interference filters only with reduced blocking properties, if at all.
As mentioned above, the pass-bands of the optical filter can be individually matched to the respective application by means of a specially designed applied layer system (e.g. an interference layer system). For example, such optical filters are used in mobile devices (e.g. smartphones), which preferably have as low a total height as possible. Optical filters are often used in integrated systems consisting of "emitters" (e.g. narrow-band LEDs or lasers) and sensors, and are intended to ensure that substantially only light from the emitters hits the sensor and extraneous light (e.g. sunlight) is blocked. The pass band of the optical filter with a high internal transmission range of preferably at least 90% should be matched as accurately as possible to the emitter used. Frequently used commercial LEDs may have their spectral maxima, e.g., 750nm, 780nm, 830nm, 850nm, 905nm, 940nm, and the like.
The optical layer according to the invention can advantageously be an interference filter layer system. Such an interference filter layer system can be designed separately in a known manner and can therefore meet various requirements. The interference filter layer system is characterized in that particularly steep flanks can be created in the transmission spectrum. Typically, multiple interference filter layers are required to produce the desired transmission properties of the filter; reference is therefore made to multilayer interference systems.
The interference layer or multilayer interference system can be applied, for example, by physical vapor deposition, PVD (german "physicikalitche gasphasenabccheidung"), for example, by thermal evaporation, sputtering, electron beam evaporation. A suitable dielectric material for forming the interference layer may be, for example, a fluoride (e.g., MgF)2、CeF3) Oxide (e.g., TiO)2、SiO2、Ta2O5) Nitrides, carbides, semiconductor materials, certain metals (in elemental form or alloys). Thin oxide layers are often used in multilayer systems for interference filters, for example as TiO layers2-SiO2Layer of TiO2Ta may also be used2O5Instead. Those skilled in the art will also recognize many other materials and methods for creating a suitable multilayer interference system on a substrate.
As an alternative or in addition to the interference filter layer, the optical filter may have an optical layer which comprises at least one absorber component. Thus, the optical filter comprises an absorbing layer. The absorbing component having suitable absorption properties is selected according to the wavelength range to be varied.
The absorbing layer may include a dye (e.g., a pigment or an organic dye) that may be present in the matrix. However, the absorbent layer may also be free of a separate matrix. The absorbing optical layer may be applied to a substrate according to the present invention, for example, by spin coating, spray coating, dip coating, casting, painting, screen printing, pad printing, ink jet printing, offset printing, roll coating, or other methods known to those skilled in the art.
The invention further provides the use of the optical filter according to the invention in the fields of distance measurement, iris recognition, gesture recognition, LIDAR (light/laser detection and ranging) applications. In particular, in these fields, systems are used which require a high internal transmission in the region of the NIR spectrum and a blocking as high as possible in the other wavelength ranges.
Table 1 below lists the specific composition (in weight%) of a Working Example (WE) of filter glass.
TABLE 1
| WE1 | WE2 | WE3 | WE4 | WE5 | WE6 | WE7 | |
| By weight% | By weight% | By weight% | By weight% | By weight% | By weight% | By weight% | |
| SiO2 | 42.72 | 42.54 | 40.54 | 42.64 | 42.91 | 40.37 | 45.54 |
| B2O3 | 2.50 | 2.70 | 2.60 | 2.80 | 1.00 | 3.20 | 0.50 |
| Al2O3 | 0.06 | 0.05 | 0.07 | 0.05 | 0.05 | 0.04 | 0.06 |
| Na2O | 0.60 | 0.40 | 0.60 | 0.50 | 0.50 | 0.70 | 0.40 |
| K2O | 21.60 | 21.90 | 22.00 | 21.80 | 24.30 | 19.30 | 21.80 |
| Rb2O | 0.04 | 0.04 | 0.04 | 0.04 | 0.04 | 0.03 | 0.04 |
| ZnO | 28.80 | 29.10 | 28.90 | 27.10 | 28.30 | 31.00 | 25.60 |
| As2O3 | 0.46 | 0.48 | 0.47 | 0.49 | 0.42 | 0.41 | 0.44 |
| Sb2O3 | 0.09 | 0.07 | 0.06 | 0.08 | 0.07 | 0.09 | 0.08 |
| CoO | 1.70 | 1.30 | 3.30 | 3.10 | 1.10 | 2.90 | 4.30 |
| CdO | 0.54 | 0.48 | 0.51 | 0.49 | 0.44 | 0.99 | 0.52 |
| SeO2 | 0.32 | 0.35 | 0.33 | 0.35 | 0.35 | 0.42 | 0.33 |
| TeO2 | 0.24 | 0.25 | 0.26 | 0.23 | 0.23 | 0.27 | 0.19 |
| SO3 | 0.16 | 0.16 | 0.16 | 0.16 | 0.16 | 0.14 | 0.08 |
| Cl | 0.17 | 0.18 | 0.16 | 0.17 | 0.13 | 0.14 | 0.12 |
| Total of | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 |
| Tg[℃] | 552 | 550 | 545 | 553 | 540 | 560 | 567 |
TABLE 1 (continue)
To produce a filter glass having a composition corresponding to working example 1, the respective glass batches were mixed vigorously. The batch materials are melted and clarified from the raw materials under reducing conditions at a temperature of about 1300 ℃ to 1360 ℃. During cooling, the glass is formed into the desired shape. The blank thus obtained is heated again (tempered) in order to form the colour. In working example 1, a two-stage annealing process was used. For nucleation, the glass is maintained at a first temperature (T) of 620 ℃ during the nucleation stagegAdd 68 ℃ C.) for 1 hour. Thereafter, the glass was heated directly to 640 ℃ (T)gA second temperature of 88 c was added to allow the desired crystallite growth (crystallite growth phase) and held at this temperature for 24 hours. In this process, the color component dissolved in the glass forms nanocrystallites (solid solution) from Cd and Zn with S, Se, Te.
In other working examples, the respective annealing temperatures are (T)g-70 ℃ to (T)g+150 ℃ and a holding time of 2-48 hours. Typically, the crystallite growth phase is preceded by a nucleation phase of 1 to 2 hours, the first temperature being chosen to be 10 ℃ to 150 ℃ lower than the second temperature. However, the nucleation stage is optional. The nucleation stage may be omitted depending on the desired position of the first transmission edge.
Drawings
The invention is further elucidated by way of example with reference to the accompanying drawing. The figures show:
FIG. 1 is an internal transmission curve of a filter glass (working example 1) of a substrate according to the present invention; and
fig. 2 is an optical filter according to the present invention.
Detailed Description
FIG. 1 shows the definition of the pass band and of the blocking range according to the invention, and the lambda of the filter glass according to the inventioni0.5The value is obtained. Lambda [ alpha ]i0.5The value describes the value of the internal transmission of the spectrum τi0.5 (corresponding to 50%). The filter glass according to the invention is defined by an internal transmission in the pass band (pass area) and an internal transmission in the blocking range. According to the invention, the pass band is understood to mean λ'i0.5And λ "i0.5The area in between. The pass band should have as high an internal transmission as possible. More specifically, in the context of the present invention, for a filter glass thickness of 0.3mm, i.e. for a wavelength range/region within the pass band, the internal transmission within the pass band should be at least 85%, preferably at least 90%, more preferably at least 91%, particularly preferably at least 95%. According to the invention, the first blocking range is understood to be the edge wavelength λ'i0.5The previous region, and the second blocking range is the edge wavelength λ "i0.5The latter region.
The blocking range should have as low an internal transmission as possible. More specifically, in the context of the present invention, for a filter glass thickness of 0.3mm, the internal transmission in the first blocking range should be at least partially, i.e. for the wavelength range in the blocking range, preferably 15% or less, preferably 10% or less, more preferably 5% or less, particularly preferably 1% or less. In the second blocking range, the internal transmission may be at most 45%, preferably at most 40%, more preferably at most 35%, further preferably at most 30%, based on the filter glass thickness, i.e. for the wavelength range in the blocking range. Preferably, the average transmission in the second blocking range may be at most 50%, preferably at most 40%, more preferably at most 30%.
As can be seen from FIG. 1, the filter glass according to the present invention (working example 1) had a thickness of 0.3mm and a bandpass propertyCan be used. With respect to internal transmittance, the filter glass has a first transmissive edge and a second transmissive edge, the first transmissive edge having an edge wavelength λ 'at 788 nm'i0.5The second transmission edge has an edge wavelength λ at 1136nm "i0.5. Between these locations there is a pass-band of the filter glass according to the invention. A section in the pass band with a particularly high internal transmission of at least 90% is obtained in the range 833nm to 959 nm. The first blocking range of the filter glass is in the wavelength range of less than 788 nm. In the first blocking range, there is an internal transmittance<1% of the segment. In this working embodiment, this high barrier has been achieved at 695nm and extends into the UV region. It can also be seen that the first transmission edge towards the short wavelength region of the spectrum rises from 10% internal transmission to 90% internal transmission in the range 712nm to 833nm, i.e. in the interval of about 120 nm. This is therefore a steep transmission edge.
Starting at a wavelength of 1136nm, the pass band is followed by a second blocking range of the filter glass. The second transmission edge towards the long-wave region of the spectrum decreases from 90% internal transmission to 25% internal transmission in the wavelength range 959nm to 1282nm and therefore does not extend as steeply as the first transmission edge. However, for many conventional applications, the internal transmission properties of the second barrier range are less important.
Fig. 2 shows the spectral transmission (solid curve) of an optical filter according to the invention. This is for example an interference band pass filter at 905 mm. Within the passband bounded by the steep edges, there is a section (about 890 to 924nm) with a particularly high spectral transmission (> 85%).
The optical filter comprised a 0.3mm thick filter glass according to the present invention (working example 1) as a substrate, and its internal transmittance was represented by a dotted curve. As the optical layer, the optical filter has a multilayer interference system whose spectral transmittance is represented by a dotted curve. It is clear that internal multilayer interference systems, in particular in the visible wavelength range, have a plurality of troublesome sub-maxima (sections with high spectral transmission). Since the filter glass according to the invention has a high blocking at wavelengths of less than 695nm, the entire optical filter also has a high blocking in this wavelength range, so that no complicated measures (for example by additional layers) are required to eliminate these sub-maxima. If the remaining sections with increased spectral transmittance (here, for example, at about 785nm, about 1073nm) which are not (completely) suppressed by the filter glass should be troublesome for the particular application, these sections may be blocked by one or more additional optical layers.
Claims (34)
1. A substrate for an optical filter comprising a filter glass containing SiO2、ZnO、K2O and cadmium chalcogenides forming a solid solution with cadmium and zinc as cationic components and sulfur, selenium and tellurium as anionic components, said filter glass being based on the oxide, TeO2In an amount of 0.1 to 3 wt%, and a CoO content of>1.0 to 7.0 wt%, wherein the filter glass has a first blocking range in the visible region of the spectrum, a passband in the near infrared region of the spectrum, a first transmission edge, and an edge wavelength λ 'between 700 and 840nm based on a filter glass thickness of 0.3 mm'i0.5Wherein the filter glass has Na in wt.% based on the oxide2O/K2Ratio of oxygen to oxygen<0.5。
2. The substrate of claim 1, wherein the filter glass at a filter glass thickness of 0.3mm has an internal transmission of less than 15% over a wavelength range between 400nm and 680 nm.
3. The substrate of claim 1, wherein the filter glass has ≦ 10% internal transmittance in a wavelength range between 400nm and 680nm at a filter glass thickness of 0.3 mm.
4. The substrate of claim 1, wherein the filter glass has ≦ 5% internal transmittance in a wavelength range between 400nm and 680nm at a filter glass thickness of 0.3 mm.
5. The substrate of claim 1, wherein the filter glass has ≦ 1% internal transmittance in a wavelength range between 400nm and 680nm at a filter glass thickness of 0.3 mm.
6. The substrate according to any one of claims 1 to 5, wherein the filter glass comprises the following composition in wt% on an oxide basis:
7. the substrate of any of claims 1-5, wherein the first transmissive edge rises from an internal transmission of 15% or less to an internal transmission of 90% or more within an interval of 150nm or less.
8. The substrate of any of claims 1-5, wherein the first transmissive edge rises from an internal transmission of 15% or less to an internal transmission of 90% or more within an interval of 130nm or less.
9. The substrate of any of claims 1-5, wherein the first transmissive edge rises from an internal transmission of 15% or less to an internal transmission of 90% or more within an interval of 120nm or less.
10. The substrate of any of claims 1-5, wherein the first transmissive edge rises from an internal transmission of 15% or less to an internal transmission of 90% or more within an interval of 110nm or less.
11. The substrate of any of claims 1-5, wherein the first transmissive edge rises from an internal transmission of 15% or less to an internal transmission of 90% or more within an interval of 100nm or less.
12. The substrate of any of claims 1-5, wherein the first transmissive edge rises from an internal transmission of 15% or less to an internal transmission of 90% or more within an interval of 80nm or less.
13. The substrate of any of claims 1-5, wherein the first transmissive edge rises from an internal transmission of 10% or less to an internal transmission of 90% or more within an interval of 150nm or less.
14. The substrate of any of claims 1-5, wherein the first transmissive edge rises from an internal transmission of 10% or less to an internal transmission of 90% or more within an interval of 130nm or less.
15. The substrate according to any one of claims 1 to 5, wherein the first transmission edge rises from an internal transmission of preferably 10% or less to an internal transmission of 90% or more within an interval of 120nm or less.
16. The substrate of any of claims 1-5, wherein the first transmissive edge rises from an internal transmission of 10% or less to an internal transmission of 90% or more within an interval of 110nm or less.
17. The substrate according to any one of claims 1 to 5, wherein the first transmission edge rises from an internal transmission of preferably 10% or less to an internal transmission of 90% or more within an interval of 100nm or less.
18. The substrate of any one of claims 1 to 5, wherein the first transmissive edge rises from an internal transmission of 10% or less to an internal transmission of 90% or more at intervals of 80nm or less.
19. The substrate according to any one of claims 1 to 5, wherein the thickness is 0.3mm, said filter glass having an internal transmission τ of at least 85% in a section of said pass bandi。
20. The substrate of any one of claims 1 to 5, wherein the filter glass has an internal transmission τ of at least 90% in a section of the pass band based on a filter glass thickness of 0.3mmi。
21. The substrate of any one of claims 1 to 5, wherein the filter glass has an internal transmission τ of at least 91% in a section of the pass band based on a filter glass thickness of 0.3mmi。
22. The substrate of any one of claims 1 to 5, wherein the filter glass has an internal transmission τ of at least 95% in a section of the pass band based on a filter glass thickness of 0.3mmi。
23. The substrate of any one of claims 1 to 5, wherein the filter glass has a second blocking range in the near infrared region, wherein there is an IR edge wavelength λ ″, based on a filter glass thickness of 0.3mm "i0.5Has an IR transmission edge between 950nm and 1300 nm.
24. The substrate according to any one of claims 1 to 5, wherein the filter glass comprises one or more of the following components in weight percent on an oxide basis:
Na2O 0-5
P2O5 0-10
TiO2 0-3
Al2O3 0-3
F 0-3
Σ RO 0-10, wherein R ═ Mg, Ca, Sr, Ba.
25. The substrate according to any one of claims 1 to 5, which isIn% by weight based on the oxides, Na of the filter glass2O/K2Ratio of oxygen to oxygen<0.3。
26. The substrate according to any one of claims 1 to 5, wherein the filter glass has Na in wt% on an oxide basis2O/K2Ratio of oxygen to oxygen<0.2。
27. The substrate according to any one of claims 1 to 5, wherein the filter glass has Na in wt% on an oxide basis2O/K2Ratio of oxygen to oxygen<0.1。
28. The substrate according to any one of claims 1 to 5, wherein the filter glass has Na in wt% on an oxide basis2O/K2Ratio of oxygen to oxygen<0.08。
29. The substrate according to any one of claims 1 to 5, wherein the filter glass has Na in wt% on an oxide basis2O/K2Ratio of oxygen to oxygen<0.05。
30. The substrate according to any one of claims 1 to 5, wherein the filter glass is free of F, and/or free of oxides of Pb, Hg, TI, Bi, Zr, Nb, Y, Yb, Gd, W, La and/or Ta, and/or free of other colouring components, and/or free of optically active components, and/or free of radioactive elements.
31. An optical filter comprising a substrate according to any of the preceding claims and at least one optical layer, wherein the at least one optical layer increases the blocking in the desired blocking range, and/or increases the steepness of the transition between the blocking range and the pass band, and/or increases the transmission in the pass band, and/or creates a narrow band pass filter.
32. The optical filter of claim 31 wherein the at least one optical layer is an interference layer system.
33. The optical filter of claim 31, wherein the at least one optical layer comprises at least one absorbing component.
34. Use of the optical filter according to any one of claims 31 to 33 in the fields of distance measurement, iris recognition, gesture recognition and LIDAR.
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| DE102017127579.7 | 2017-11-22 | ||
| DE102017127579.7A DE102017127579B3 (en) | 2017-11-22 | 2017-11-22 | Substrate for an optical filter and optical filter |
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| KR20210023565A (en) * | 2019-08-23 | 2021-03-04 | 현대자동차주식회사 | Optic filter integrated with lidar window |
| CN110837145B (en) * | 2019-11-21 | 2022-03-29 | 天津津航技术物理研究所 | Method for regulating and controlling spectrum of narrow-band filter |
| DE102022121122A1 (en) | 2022-08-22 | 2024-02-22 | Schott Ag | Laminated glass and its use |
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| KR102001788B1 (en) | 2019-07-18 |
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