CN114195383A - Preparation process of blue glass for infrared cut-off filter - Google Patents
Preparation process of blue glass for infrared cut-off filter Download PDFInfo
- Publication number
- CN114195383A CN114195383A CN202111617138.2A CN202111617138A CN114195383A CN 114195383 A CN114195383 A CN 114195383A CN 202111617138 A CN202111617138 A CN 202111617138A CN 114195383 A CN114195383 A CN 114195383A
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- glass
- blue glass
- infrared cut
- blue
- filter
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- 239000011521 glass Substances 0.000 title claims abstract description 136
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 23
- FGDZQCVHDSGLHJ-UHFFFAOYSA-M rubidium chloride Inorganic materials [Cl-].[Rb+] FGDZQCVHDSGLHJ-UHFFFAOYSA-M 0.000 claims abstract description 21
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims abstract description 11
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 9
- 229910003069 TeO2 Inorganic materials 0.000 claims abstract description 8
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003086 colorant Substances 0.000 claims abstract description 7
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 239000008395 clarifying agent Substances 0.000 claims abstract description 4
- 239000005751 Copper oxide Substances 0.000 claims abstract description 3
- 229910000431 copper oxide Inorganic materials 0.000 claims abstract description 3
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 18
- 239000000758 substrate Substances 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 11
- 229910052681 coesite Inorganic materials 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 229910052906 cristobalite Inorganic materials 0.000 claims description 10
- 239000000377 silicon dioxide Substances 0.000 claims description 10
- 229910052682 stishovite Inorganic materials 0.000 claims description 10
- 229910052905 tridymite Inorganic materials 0.000 claims description 10
- 239000006060 molten glass Substances 0.000 claims description 9
- 238000009423 ventilation Methods 0.000 claims description 9
- 239000000156 glass melt Substances 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 239000002131 composite material Substances 0.000 claims description 7
- 229910009815 Ti3O5 Inorganic materials 0.000 claims description 6
- 239000006121 base glass Substances 0.000 claims description 6
- 238000005352 clarification Methods 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 5
- 239000006025 fining agent Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000002844 melting Methods 0.000 abstract description 7
- 230000008018 melting Effects 0.000 abstract description 7
- 230000007547 defect Effects 0.000 abstract description 2
- 239000005304 optical glass Substances 0.000 abstract description 2
- 238000005266 casting Methods 0.000 abstract 2
- 238000002156 mixing Methods 0.000 description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 24
- 238000003756 stirring Methods 0.000 description 21
- 238000002834 transmittance Methods 0.000 description 21
- 238000005259 measurement Methods 0.000 description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 12
- 238000002791 soaking Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- 238000004506 ultrasonic cleaning Methods 0.000 description 12
- 238000005406 washing Methods 0.000 description 12
- XUJLWPFSUCHPQL-UHFFFAOYSA-N 11-methyldodecan-1-ol Chemical compound CC(C)CCCCCCCCCCO XUJLWPFSUCHPQL-UHFFFAOYSA-N 0.000 description 9
- XLSMFKSTNGKWQX-UHFFFAOYSA-N hydroxyacetone Chemical compound CC(=O)CO XLSMFKSTNGKWQX-UHFFFAOYSA-N 0.000 description 9
- 238000004140 cleaning Methods 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
- 150000002500 ions Chemical class 0.000 description 8
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 description 8
- 229940069446 magnesium acetate Drugs 0.000 description 8
- 235000011285 magnesium acetate Nutrition 0.000 description 8
- 239000011654 magnesium acetate Substances 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 230000032683 aging Effects 0.000 description 7
- 238000007789 sealing Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000005520 cutting process Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000003599 detergent Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Natural products CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 235000019589 hardness Nutrition 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 229940102127 rubidium chloride Drugs 0.000 description 4
- 239000003381 stabilizer Substances 0.000 description 4
- 238000012876 topography Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910001597 celsian Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- 239000002245 particle Substances 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Images
Classifications
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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
- C03C4/02—Compositions for glass with special properties for coloured glass
-
- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/004—Refining agents
-
- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/04—Opacifiers, e.g. fluorides or phosphates; Pigments
-
- 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
-
- 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
- C03C4/082—Compositions for glass with special properties for glass selectively absorbing radiation of specified wave lengths for infrared absorbing glass
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Abstract
The invention provides a preparation process of blue glass for an infrared cut-off filter, belonging to the field of optical glass2、Na2O and CaO; the clarifying agent comprises Sb2O3RbCl and TeO2(ii) a The colorant comprises copper oxide; melting and casting glass raw materials to obtain a glass precursor, and melting, clarifying and casting the glass precursor to obtain the blue glass. The invention provides a preparation method of blue glass for an infrared cut-off filterThe method has the advantages of low production consumption, few product defects, good mechanical property and wide application range.
Description
Technical Field
The invention belongs to the field of optical glass, and particularly relates to a preparation process of blue glass for an infrared cut-off filter.
Background
Any object can emit infrared rays outwards under the environment of more than absolute zero degree; the camera of the mobile phone adopts CCD or CMOS sensors; CCD and CMOS sensors can sensitively capture all visible and part of infrared light. The principle and law of refraction of light can be used to derive: the longer the wavelength, the smaller the refractive index; the shorter the wavelength, the larger the refractive index. Therefore, when the light rays enter the camera of the mobile phone and are refracted by the lens of the lens, the visible light and the infrared light can form images on different target surfaces. Where the visible light is imaged as a color image and the infrared light is imaged as a black and white image. When we adjust the image formed by visible light, namely, the image focusing and back focus adjustment, the infrared light forms a virtual image on the target surface, thereby affecting the color and quality of the image.
To avoid the virtual image of the target surface caused by infrared light, the most effective means at present is to filter out the infrared light by IRCoating film or adding an optical filter, and reduce the real color of the object, thereby solving the problem of color distortion of the image. The blue glass differs from other filters in the raw material. The blue glass is made of a blue glass material, and has the effect of filtering infrared light in an absorption mode. The blue light has higher penetration rate than red-orange glass filter, so that the glass filter has better penetration rate, can filter infrared light above 630nm, and can filter the infrared light more thoroughly.
The prior art discloses a thick blue glass formula for an infrared cut-off filter, such as a Chinese patent with an issued publication number of CN 103058519B, and the formula comprises 50-70 wt% of a glass network structure forming agent, 8-22 wt% of a weather-resistant stabilizer, 0.3-3 wt% of a glass stabilizer, 10-25 wt% of a softening stabilizer, 0-1.5 wt% of a defoaming clarifier, 2-10 wt% of a hardness-improving stabilizer, 0-15 wt% of a fluxing agent and 2.5-5 wt% of a near-infrared cut-off coloring agent; compared with the prior art, the obtained blue glass for the infrared cut-off filter has the light transmittance of more than 87% in a visible light region, has the light transmittance of less than 3% in an infrared cut-off part, and can be stable for 1000 hours in an environment with the temperature of 85 ℃ and the humidity of 90%.
Disclosure of Invention
The invention aims to provide a preparation method of blue glass for an infrared cut-off filter, which can promote the elimination of bubbles in glass liquid, simplify the operation and improve the yield of glass production, and the prepared product has better mechanical property and wider application range.
The technical scheme adopted by the invention for realizing the purpose is as follows:
the preparation method of the blue glass for the infrared cut-off filter comprises the following steps:
s1, the blue glass raw material comprises a basic glass composition, a clarifying agent and a coloring agent, wherein the basic glass composition mainly comprises SiO2、Na2O and CaO; the clarifying agent comprises Sb2O3RbCl and TeO2(ii) a The colorant comprises copper oxide;
s2, starting the high-temperature lifting furnace, heating to 1350-1450 ℃ at the speed of 50-100 ℃/h, adding the blue glass raw material into the crucible, placing the crucible into the high-temperature lifting furnace, introducing protective gas into the furnace according to the ventilation quantity of 20-50L/h, preserving the temperature for 20-40min to obtain glass melt, and introducing the protective gas into the glass melt according to the ventilation quantity of 100 plus 150L/h;
s3, cooling the high-temperature lifting furnace to 1250-;
s4, heating the high-temperature lifting furnace to 1400-1500 ℃ at the speed of 50-100 ℃/h, breaking the glass precursor, adding the broken glass precursor into the crucible, placing the crucible in the high-temperature lifting furnace, and introducing protective gas according to the ventilation quantity of 50-100L/h;
s5, heating the high-temperature lifting furnace to 1450-1600 ℃ at the speed of 30-60 ℃/h, and preserving the temperature for 10-15h to ensure that the molten glass enters a clarification stage;
s6, cooling the high-temperature lifting furnace to 1350-. The high-temperature viscosity of the glass melt prepared by melting the blue glass raw material added with rubidium chloride and tellurium dioxide is low, so that the removal of bubbles in glass liquid is facilitated, the visible bubbles in the prepared blue glass are few, and the prepared blue glass has good mechanical properties, the application range of the product is widened, and the application prospect is good.
In some embodiments, the shielding gas is a mixture of nitrogen and oxygen.
In some embodiments, the base glass composition comprises: 66-75 parts by weight of SiO210-20 parts by weight of Na2O, 5-15 parts by weight of CaO, 0-5 parts by weight of MgO and 0-5 parts by weight of Al2O30 to 5 parts by weight of K2O。
In some embodiments, the fining agent is present in an amount ranging from 0 to 0.6 wt% of the base glass composition.
In some embodiments, the above fining agent comprises the following components in parts by weight: 50-60 parts by weight of Sb2O310-20 parts of RbCl and 5-10 parts of TeO2。
In some embodiments, the colorant is present in an amount of 2 to 6.5 weight percent of the base glass composition.
The blue glass is prepared by the preparation method of the blue glass for the infrared cut-off filter.
The application of the blue glass in preparing the infrared cut-off filter is provided.
Another object of the present invention is to provide a method for manufacturing an infrared cut-off filter, which can improve the transmittance and mechanical properties of the infrared cut-off filter in a visible light region, and improve the service life of the product.
The technical scheme adopted by the invention for realizing the purpose is as follows:
provided is a method for manufacturing an infrared cut filter, including: the blue glass substrate is prepared by adopting the preparation method of the blue glass for the infrared cut-off filter, the buffer layer is arranged on the blue glass substrate, and the composite film layer is arranged outside the buffer layer.
In some embodiments, the composite film layer is made of a high refractive index material Ti3O5And low refractive index material SiO2And alternately overlapping.
In some embodiments, the buffer layer is made of MgF2+Al2O3Or MgF2A film layer of material. From MgF2+Al2O3Or MgF2The buffer layer made of the material can be well combined with the substrate, and the combination capability of the composite film layer is improved.
In some embodiments, the coating method of the composite film layer comprises: ti on the buffer layer3O5And SiO2Repeating alternating stack deposition with ion source assistance; wherein, Ti3O5The auxiliary energy of the ion source is BV: 800-1100V, IB: 700 and 1200 mA; SiO 22The auxiliary energy of the ion source is BV: 700-1100V, IB: 700- > 1100 mA;
in some embodiments, the above Ti3O5When the material is coated, the vacuum degree is 0.018-0.022Pa, the film forming rate is 0.2-0.4nm/s, the thickness is 40-150nm, and the deflection current of an electron gun is 380-; the above SiO2When the material is used for coating, the vacuum degree is 0.011-0.014Pa, the film forming rate is 1.0-1.4nm/s, the thickness is 80-180nm, and the deflection current of an electron gun is 155-165 mA.
In some embodiments, the above is made of MgF2The coating method of the buffer layer made of the material is a sol-gel method.
In some embodiments, the above is made of MgF2The coating method of the buffer layer made of the material specifically comprises the following steps:
immersing the above blue glass substrate in MgF2Standing and staying in the sol for 1-3min, then pulling the blue glass substrate out of the sol at a pulling speed of 14-16cm/min, drying, and then placing into a muffle furnace for heat treatment, wherein the heat treatment process parameters are as follows: the heating rate is 4-8 ℃/min, the heat treatment temperature is 520-530 ℃, and the heat preservation time is 1-2 h.
In some embodiments, the above MgF2The preparation method of the sol comprises the following steps: mixing magnesium acetate with anhydrous ethyl acetateMixing alcohol, and stirring at normal temperature for 30min to obtain solution A; mixing hydrofluoric acid and absolute ethyl alcohol, and stirring at normal temperature for 30min to obtain a solution B; mixing the solution A and the solution B, stirring at the constant temperature of 40 ℃ for 20h, sealing and aging for 15-25h to obtain MgF2And (3) sol.
In some embodiments, the molar ratio of magnesium acetate to absolute ethanol in solution a is from 1:20 to 30.
In some embodiments, the molar ratio of hydrofluoric acid to absolute ethanol in solution B is 1: 10-15.
In some embodiments, the solution B further includes isotridecanol and acetol.
In some embodiments, the ratio of absolute ethanol in solution B: the molar ratio of isotridecanol to acetol is 10-20:2-5: 4-8. MgF2The addition of isotridecyl alcohol and acetol in the sol can improve MgF2The porosity and the aperture of the film are uniformly distributed, the obtained film is compact, the prepared coated blue glass has high visible light transmittance and excellent hardness, the use experience of the product is optimized, and the service life of the product is prolonged.
The invention has the following beneficial effects because the rubidium chloride and the tellurium dioxide are added into the blue glass raw material: the high-temperature viscosity of the molten glass is low, which is beneficial to removing bubbles in the glass liquid, so that the produced blue glass has less visible bubbles and good mechanical property.
Therefore, the preparation method of the blue glass for the infrared cut-off filter has the advantages of low production consumption, few product defects, good mechanical property and wide application range.
The invention is used for preparing MgF2When the sol is added, isotridecanol and acetol are added, so that the sol has the following beneficial effects: can improve MgF2The porosity and the pore diameter of the film are uniformly distributed, the obtained film is compact, and the prepared coated blue glass has high visible light region light transmittance and excellent hardness.
Therefore, the invention is a preparation method of the infrared cut-off filter with high visible light transmittance, good mechanical property and long service life.
Drawings
FIG. 1 is a graph showing the results of viscosity measurement in test example 1 of the present invention;
FIG. 2 is a result of measurement of the escape rate of bubbles in test example 1 of the present invention;
FIG. 3 is a graph showing the results of measurement of microhardness in test example 1 of the present invention;
FIG. 4 is a graph showing the results of measurement of flexural strength in test example 1 of the present invention;
FIG. 5 is a result of measurement of porosity in test example 2 of the present invention;
FIG. 6 shows MgF in test example 2 of the present invention2The surface topography of the film;
FIG. 7 is a result of measurement of light transmittance in test example 2 of the present invention;
FIG. 8 is a graph showing the results of measurement of microhardness in test example 2 of the present invention.
Detailed Description
The present invention is further described in detail with reference to the following examples:
example 1:
1. a preparation process of blue glass for an infrared cut-off filter specifically comprises the following steps:
1.1 mixing 140g of SiO2、30g Na2O、20g CaO、8g MgO、10g Al2O3、6gK2O、0.75g Sb2O3、0.22g RbCl、0.10g TeO2And 11.8g of CuO were uniformly mixed to obtain a blue glass raw material.
1.2 starting the high-temperature lifting furnace, heating to 1400 ℃ at the speed of 80 ℃/h, adding 120g of blue glass raw material into an alumina crucible, placing the alumina crucible in the high-temperature lifting furnace, simultaneously introducing mixed gas of 40 v/v% nitrogen and 60 v/v% oxygen into the furnace according to the ventilation quantity of 30L/h, adding 54g of blue glass raw material residual material after 15min, finishing adding the residual material after 15min, preserving heat for 25min to obtain glass melt, and introducing mixed gas of 40 v/v% nitrogen and 60 v/v% oxygen into the glass melt according to the ventilation quantity of 120L/h.
1.3, cooling the high-temperature lifting furnace to 1300 ℃ at the speed of 5 ℃/min, preserving the temperature for 2h, stopping introducing mixed gas of 40 v/v% nitrogen and 60 v/v% oxygen into the molten glass, pouring the molten glass into a cast iron mould with water cooling, and naturally cooling to room temperature to obtain the glass precursor.
1.4 heating the high-temperature lifting furnace to 1450 ℃ at the speed of 80 ℃/h, breaking the glass precursor, adding the glass precursor into a platinum crucible, placing the platinum crucible into the high-temperature lifting furnace, and simultaneously introducing mixed gas of 40 v/v% nitrogen and 60 v/v% oxygen according to the ventilation quantity of 80L/h.
1.5 heating the high-temperature lifting furnace to 1550 ℃ at the speed of 50 ℃/h, and preserving the heat for 13h to ensure that the molten glass enters a clarification stage.
1.6 cooling the high-temperature lifting furnace to 1400 ℃ at the speed of 80 ℃/h, stirring the molten glass at the rotating speed of 30r/min for 12h, cooling the rotating speed to 6r/min, pouring the molten glass into a graphite mold, quickly moving the graphite mold into an annealing furnace, and annealing at 500 ℃ for 85h to obtain the formed blue glass. The obtained blue glass was cut to a thickness of 1mm, and had a transmittance of 83.7% at a wavelength of 400nm, a transmittance of 88.9% at a wavelength of 500nm, a transmittance of 87.3% at a wavelength of 600nm, a transmittance of 16.5% at a wavelength of 700nm, a transmittance of 15.8% at a wavelength of 800nm, a transmittance of 19.3% at a wavelength of 900nm, a transmittance of 21.7% at a wavelength of 1000nm, and a transmittance of 23.6% at 1100 nm.
Example 2:
1. a method for preparing an infrared cut filter includes:
1.1 cleaning of blue glass substrate: cutting the blue glass sheet prepared by the method of the embodiment 1 into the specification of 10mm multiplied by 1mm, washing the blue glass sheet once by using detergent, washing the blue glass sheet by using deionized water, soaking the blue glass sheet by using acetone, and carrying out ultrasonic cleaning for 30 min; soaking in anhydrous ethanol, and ultrasonic cleaning for 30 min.
1.2MgF2Preparing sol: mixing 1mol of magnesium acetate with 25mol of absolute ethyl alcohol, and magnetically stirring at normal temperature for 30min to obtain a solution A; mixing 2.1mol of hydrofluoric acid, 20mol of absolute ethyl alcohol, 4mol of isotridecanol and 6.7mol of acetone alcohol, and magnetically stirring at normal temperature for 30min to obtain a solution B; mixing the solution A and the solution B, stirring at the constant temperature of 40 ℃ for 20h, sealing and aging for 20h to obtain MgF2And (3) sol.
1.3MgF2Preparing a film layer: immersing the cleaned blue glass substrate into MgF2Standing and staying in the sol for 2min, then pulling the blue glass substrate out of the sol at the pulling speed of 15cm/min, drying at 35 ℃, and then placing the substrate into a muffle furnace for heat treatment, wherein the heat treatment process parameters are as follows: the heating rate is 4 ℃/min, the heat treatment temperature is 525 ℃, the heat preservation time is 1h, and MgF is plated2The blue glass matrix of the film.
1.4 preparation of composite film layer: forming 10 Ti layers on the buffer layer3O5Film layer and 10 layers of SiO2The film layers are repeatedly and alternately stacked and deposited under the assistance of an ion source, and Ti3O5The material is deposited using an ion source assisted deposition with an ion source assist energy of: BV: 1000V, IB: 800mA, Ti3O5When the material is coated, the vacuum degree is 0.02Pa, the film forming rate is 0.3nm/s, the thickness is 80nm, and the deflection current of an electron gun is 390 mA; SiO 22The material is deposited using an ion source assisted deposition with an ion source assist energy of: BV: 900V, IB: 800mA, SiO2When the material is coated, the vacuum degree is 0.015Pa, the film forming rate is 1.5nm/s, the thickness is 100nm, and the deflection current of an electron gun is 160mA, so that the infrared cut-off filter is obtained.
Example 3:
1. a preparation process of blue glass for an infrared cut-off filter specifically comprises the following steps:
1.1 mixing 140g of SiO2、30g Na2O、20g CaO、8g MgO、10g Al2O3、6gK2O、0.75g Sb2O3、0.16g RbCl、0.12g TeO2And 11.8g of CuO were uniformly mixed to obtain a blue glass raw material. The rest of the description is identical to example 1.
Example 4:
1. a preparation process of blue glass for an infrared cut-off filter specifically comprises the following steps:
1.1 mixing 140g of SiO2、30g Na2O、20g CaO、8g MgO、10g Al2O3、6gK2O、0.75g Sb2O3、0.25g RbCl、0.08g TeO211.8g of CuO were mixed wellAnd obtaining the blue glass raw material. The rest of the description is identical to example 1.
Example 5:
1. a preparation process of blue glass for an infrared cut-off filter specifically comprises the following steps:
1.1 mixing 140g of SiO2、30g Na2O、20g CaO、8g MgO、10g Al2O3、6gK2O、0.75g Sb2O30.22g of RbCl and 11.8g of CuO are uniformly mixed to obtain a blue glass raw material. The rest of the description is identical to example 1.
Example 6:
1. a preparation process of blue glass for an infrared cut-off filter specifically comprises the following steps:
1.1 mixing 140g of SiO2、30g Na2O、20g CaO、8g MgO、10g Al2O3、6gK2O、0.75g Sb2O3、0.10g TeO2And 11.8g of CuO were uniformly mixed to obtain a blue glass raw material. The rest of the description is identical to example 1.
Example 7:
1. a preparation process of blue glass for an infrared cut-off filter specifically comprises the following steps:
1.1 mixing 140g of SiO2、30g Na2O、20g CaO、8g MgO、10g Al2O3、6gK2O、0.75g Sb2O3And 11.8g of CuO are uniformly mixed to obtain the blue glass raw material. The rest of the description is identical to example 1.
Example 8:
1. a method for preparing an infrared cut filter includes:
1.1 cleaning of blue glass substrate: cutting the blue glass sheet prepared by the method of the embodiment 1 into the specification of 10mm multiplied by 1mm, washing the blue glass sheet once by using detergent, washing the blue glass sheet by using deionized water, soaking the blue glass sheet by using acetone, and carrying out ultrasonic cleaning for 30 min; soaking in anhydrous ethanol, and ultrasonic cleaning for 30 min.
1.2MgF2Preparing sol: mixing 1mol of magnesium acetate with 25mol of absolute ethyl alcohol, and magnetically stirring at normal temperature for 30min to obtain a solution A; 2.1mol of hydrofluoric acid and 20mol of hydrofluoric acidAbsolute ethyl alcohol, 4.4mol of isotridecyl alcohol and 7.8mol of acetone alcohol are mixed, and the mixture is magnetically stirred for 30min at normal temperature to obtain solution B; mixing the solution A and the solution B, stirring at the constant temperature of 40 ℃ for 20h, sealing and aging for 20h to obtain MgF2And (3) sol. The rest of the description is identical to example 2.
Example 9:
1. a method for preparing an infrared cut filter includes:
1.1 cleaning of blue glass substrate: cutting the blue glass sheet prepared by the method of the embodiment 1 into the specification of 10mm multiplied by 1mm, washing the blue glass sheet once by using detergent, washing the blue glass sheet by using deionized water, soaking the blue glass sheet by using acetone, and carrying out ultrasonic cleaning for 30 min; soaking in anhydrous ethanol, and ultrasonic cleaning for 30 min.
1.2 MgF2Preparing sol: mixing 1mol of magnesium acetate with 25mol of absolute ethyl alcohol, and magnetically stirring at normal temperature for 30min to obtain a solution A; mixing 2.1mol of hydrofluoric acid, 20mol of absolute ethyl alcohol, 6.5mol of isotridecanol and 8mol of acetone alcohol, and magnetically stirring at normal temperature for 30min to obtain a solution B; mixing the solution A and the solution B, stirring at the constant temperature of 40 ℃ for 20h, sealing and aging for 20h to obtain MgF2And (3) sol. The rest of the description is identical to example 2.
Example 10:
1. a method for preparing an infrared cut filter includes:
1.1 cleaning of blue glass substrate: cutting the blue glass sheet prepared by the method of the embodiment 1 into the specification of 10mm multiplied by 1mm, washing the blue glass sheet once by using detergent, washing the blue glass sheet by using deionized water, soaking the blue glass sheet by using acetone, and carrying out ultrasonic cleaning for 30 min; soaking in anhydrous ethanol, and ultrasonic cleaning for 30 min.
1.2MgF2Preparing sol: mixing 1mol of magnesium acetate with 25mol of absolute ethyl alcohol, and magnetically stirring at normal temperature for 30min to obtain a solution A; mixing 2.1mol of hydrofluoric acid, 20mol of absolute ethyl alcohol and 4mol of isotridecanol, and magnetically stirring at normal temperature for 30min to obtain a solution B; mixing the solution A and the solution B, stirring at the constant temperature of 40 ℃ for 20h, sealing and aging for 20h to obtain MgF2And (3) sol. The rest of the description is identical to example 2.
Example 11:
1. a method for preparing an infrared cut filter includes:
1.1 cleaning of blue glass substrate: cutting the blue glass sheet prepared by the method of the embodiment 1 into the specification of 10mm multiplied by 1mm, washing the blue glass sheet once by using detergent, washing the blue glass sheet by using deionized water, soaking the blue glass sheet by using acetone, and carrying out ultrasonic cleaning for 30 min; soaking in anhydrous ethanol, and ultrasonic cleaning for 30 min.
1.2 MgF2Preparing sol: mixing 1mol of magnesium acetate with 25mol of absolute ethyl alcohol, and magnetically stirring at normal temperature for 30min to obtain a solution A; mixing 2.1mol of hydrofluoric acid, 20mol of absolute ethyl alcohol and 6.7mol of acetone alcohol, and magnetically stirring at normal temperature for 30min to obtain a solution B; mixing the solution A and the solution B, stirring at the constant temperature of 40 ℃ for 20h, sealing and aging for 20h to obtain MgF2And (3) sol. The rest of the description is identical to example 2.
Example 12:
1. a method for preparing an infrared cut filter includes:
1.1 cleaning of blue glass substrate: cutting the blue glass sheet prepared by the method of the embodiment 1 into the specification of 10mm multiplied by 1mm, washing the blue glass sheet once by using detergent, washing the blue glass sheet by using deionized water, soaking the blue glass sheet by using acetone, and carrying out ultrasonic cleaning for 30 min; soaking in anhydrous ethanol, and ultrasonic cleaning for 30 min.
1.2 MgF2Preparing sol: mixing 1mol of magnesium acetate with 25mol of absolute ethyl alcohol, and magnetically stirring at normal temperature for 30min to obtain a solution A; mixing 2.1mol of hydrofluoric acid and 20mol of absolute ethyl alcohol, and magnetically stirring at normal temperature for 30min to obtain a solution B; mixing the solution A and the solution B, stirring at the constant temperature of 40 ℃ for 20h, sealing and aging for 20h to obtain MgF2And (3) sol. The rest of the description is identical to example 2.
Test example 1:
1.1 viscosity analysis: a blue glass sample with the particle size of 1mm is tested by using a RSV1700 high-temperature viscometer produced by ORTON in America under the same condition to obtain viscosity values at different temperatures, and a graph is obtained by data analysis and processing. The results of the viscosity measurements are shown in FIG. 1.
1.2 bubble observation: analysis using CelSian high temperature observation system: and respectively feeding the blue glass raw materials in the above embodiments into a quartz tube, heating to 1600 ℃, preserving heat for 1.5h, then cooling to 1100 ℃ within 1.5h, and taking out the quartz tube to finish the experiment. Through the analysis and processing of the collected pictures, the dynamic condition of the bubble change in the raw material melting process is recorded, and 15 bubbles which can completely observe the motion trail of the raw material are selected. The escape rate of bubbles during the temperature increase of 1200 ℃ to 1500 ℃ was observed. The results of the measurement of the bubble evolution rate are shown in FIG. 2.
1.3 clarification effect analysis: the blue glass samples prepared in the above examples using different fining agents were cut into 50mm × 50mm × 10mm thin pieces, and the surfaces of the glass pieces were finely ground and polished. The number and diameter of the bubbles were observed in the obtained glass sheet using a Nikon polarizing microscope of Eclipse LV100 POL. The clarification effect of the different clarifiers is shown in table 1.
TABLE 1 clarification Effect of different clarifiers
| Group of | Total number of bubbles (number) | Average diameter of air bubble (mm) | Total volume of bubbles/volume of glass (ppm) |
| Example 1 | 7 | 0.1965 | 157 |
| Example 3 | 8 | 0.1978 | 165 |
| Example 4 | 8 | 0.1989 | 172 |
| Example 5 | 15 | 0.2466 | 395 |
| Example 6 | 19 | 0.2662 | 502 |
| Example 7 | 21 | 0.2675 | 511 |
1.4 determination of mechanical Properties of blue glass:
the blue glass samples obtained in the above examples were each cut into 35mm × 22mm × 1mm thin pieces and tested for mechanical properties.
1.4.1 measurement of microhardness: and measuring the microhardness of the sample by using an HVS-1000 type digital display microhardness meter. A Vickers diamond pressure head is adopted, the load is 0.981N, and the loading time is 10 s. Five points were taken for each sample and the measured values were averaged.
1.4.2 determination of flexural Strength: the commonly used three-point bending test method is adopted, and an RGM-4100 electronic universal tester produced by Shenzhen Rungel instruments Limited is used for testing the flexural strength of the blue glass sample. The results of the microhardness measurements are shown in FIG. 3. The results of the flexural strength measurements are shown in FIG. 4.
As can be seen from fig. 1, the high temperature viscosity of the blue glass prepared by melting the raw materials of examples 1, 3 and 4 is lower than that of examples 5, 6 and 7, and as can be seen from fig. 2, the bubble escape rate of the raw materials of examples 1, 3 and 4 during melting is higher than that of examples 5, 6 and 7, and as can be seen from table 1, the bubble number, the bubble diameter and the ratio of the total bubble volume to the glass volume of the blue glass prepared by melting the raw materials of the blue glass added with rubidium chloride and tellurium dioxide are all lower than those of the blue glass prepared, which shows that the high temperature viscosity of the glass melt prepared by melting the blue glass raw materials added with rubidium chloride and tellurium dioxide is lower, which is beneficial to the elimination of bubbles in the molten glass, so that the blue glass prepared has fewer visible bubbles and thus better mechanical properties.
Test example 2:
2.1 MgF2determination of film porosity: the MgF prepared in the above example was analyzed by a specific surface area analyzer2The film is tested, the sample is in a solid gel state, the main principle is that the cavity is filled with nitrogen, the filled nitrogen can be adsorbed on pores, and the porosity of the sample is obtained by calculating the adsorption and desorption volumes of the nitrogen. The results of the porosity measurement are shown in FIG. 5.
2.2 surface topography analysis: the MgF of examples 2 and 12 was analyzed by field emission scanning electron microscopy of the type ULTRA PLUS, produced by Zeiss, Germany2Surface topography of the film. MgF2The surface topography of the film is shown in FIG. 6.
2.3 MgF was plated in the above examples using UV-VIS spectrophotometer model Uv-2420 manufactured by Shimadzu corporation of Japan2The blue glass matrix of the film was tested for light transmittance. The specific operation is as follows: preheat spectrophotometer for 30min, take out the cell frame wherein, adopt self-control slide glass to measure the base, in fixing and inserting spectrophotometer's light path perpendicularly automatically cleaning glass piece, let light vertical irradiation automatically cleaning glass piece, cover the top cap, wait to record down data after the numerical value of luminousness is stable. The distance between the glass sheet and the light transmission opening needs to be kept consistent in each measurement so as to reduce measurement errors. Measured at wavelengths of 400, 450, 500, 550 and 600nm, respectivelyMgF2Transmittance of blue glass of the film, 3 transmittance measurements were made for each glass sheet, and the average value was taken as the final result. The measurement results of the light transmittance are shown in FIG. 7.
2.4 testing MgF plated in the above examples on a HVS-1000 type digital display microhardness tester2The microhardness of the blue glass substrate sample of the film is 0.981N under the load of a Vickers diamond pressure head for 10 s. Five points were taken for each sample and the measured values were averaged. The results of the microhardness measurements are shown in FIG. 8.
As can be seen from FIG. 5, MgF of examples 2, 8 and 92The film porosity was greater than that of examples 10, 11 and 12, and it can be seen from FIG. 6 that MgF produced in example 2 was comparable to that of example 122The films had uniform pore size distribution, no cracks, and were relatively dense, as can be seen from FIG. 7, the light transmittances of examples 2, 8, and 9 were greater than those of examples 10, 11, and 12, and from FIG. 8, the hardnesses of examples 2, 8, and 9 were greater than those of examples 10, 11, and 12, which indicates that MgF is present2The addition of isotridecyl alcohol and acetol in the sol can improve MgF2The porosity and the pore diameter of the film are uniformly distributed, and the obtained film is compact, so that the light transmittance and the hardness of the blue glass in a visible light area can be improved.
Conventional techniques in the above embodiments are known to those skilled in the art, and therefore, will not be described in detail herein.
The above embodiments are merely illustrative, and not restrictive, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention. Therefore, all equivalent technical solutions also belong to the scope of the present invention, and the protection scope of the present invention should be defined by the claims.
Claims (8)
1. A preparation method of blue glass for an infrared cut-off filter is characterized by specifically comprising the following steps:
s1 blue glass raw material comprising basic glass composition and clarificationAn agent and a colorant, wherein the base glass composition mainly comprises SiO2、Na2O and CaO; the clarifying agent comprises Sb2O3RbCl and TeO2(ii) a The colorant comprises copper oxide;
s2, starting the high-temperature lifting furnace, heating to 1350-1450 ℃ at the speed of 50-100 ℃/h, adding the blue glass raw material into the crucible, placing the crucible into the high-temperature lifting furnace, introducing protective gas into the furnace according to the ventilation quantity of 20-50L/h, preserving the temperature for 20-40min to obtain glass melt, and introducing the protective gas into the glass melt according to the ventilation quantity of 100 plus 150L/h;
s3, cooling the high-temperature lifting furnace to 1250-;
s4, heating the high-temperature lifting furnace to 1400-1500 ℃ at the speed of 50-100 ℃/h, breaking the glass precursor, adding the broken glass precursor into the crucible, placing the crucible in the high-temperature lifting furnace, and introducing protective gas according to the ventilation quantity of 50-100L/h;
s5, heating the high-temperature lifting furnace to 1450-1600 ℃ at the speed of 30-60 ℃/h, and preserving the temperature for 10-15h to ensure that the molten glass enters a clarification stage;
s6, cooling the high-temperature lifting furnace to 1350-.
2. The method of claim 1, wherein: the base glass composition includes: 66-75 parts by weight of SiO210-20 parts by weight of Na2O, 5-15 parts by weight of CaO, 0-5 parts by weight of MgO and 0-5 parts by weight of Al2O30 to 5 parts by weight of K2O。
3. The method of claim 1, wherein: the fining agent is present in an amount ranging from 0 to 0.6 wt% of the base glass composition.
4. A blue glass, characterized in that: the blue glass for an infrared cut filter, which is produced by the process for producing a blue glass for an infrared cut filter according to any one of claims 1 to 3.
5. Use of a blue glass according to claim 4 for the preparation of an infrared cut filter.
6. A method for manufacturing an infrared cut filter is characterized by comprising the following steps: the blue glass substrate is prepared by the method for preparing the blue glass for the infrared cut-off filter, which is described in any one of claims 1 to 3, wherein a buffer layer is arranged on the blue glass substrate, and a composite film layer is arranged outside the buffer layer.
7. The method according to claim 6, wherein: the composite film layer is made of high-refractive-index material Ti3O5And low refractive index material SiO2And alternately overlapping.
8. The method according to claim 6, wherein: the buffer layer is made of MgF2+Al2O3Or MgF2A film layer of material.
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