CN102432174A - Infrared window glass - Google Patents
Infrared window glass Download PDFInfo
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- CN102432174A CN102432174A CN2011102646240A CN201110264624A CN102432174A CN 102432174 A CN102432174 A CN 102432174A CN 2011102646240 A CN2011102646240 A CN 2011102646240A CN 201110264624 A CN201110264624 A CN 201110264624A CN 102432174 A CN102432174 A CN 102432174A
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- glass
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- window
- infrared window
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Abstract
The invention relates to infrared window glass, which is mainly composed of 15-25 of GeO2, 15-25 of Ga2O3, 30-45 of MO, 5-10 of Al2O3, 1-5 of BaCl2, and 5-15 of N2CO3. The infrared window glass of the invention is especially suitable for high temperature surface heat treatment and bonding with another infrared material (germinate infrared glass, sapphire crystals, etc.), and a metal grid can be added between them so as to form a high transparent infrared window.
Description
Technical field
The present invention relates to a kind of infrared window glass, particularly be fit to and another kind of infra-red material (germanate infrared glass, white gem crystal etc.) high temperature surface thermal treatment bonding, the middle metal grill that adds forms a kind of high transparent infrared window that contains electro-magnetic screen function.
Technical background
The spectrum of many transmitters or the employed material of laser system is in visible-middle infra-red range (0.5~5 μ m).A protection of these system requirements window, and the size of window, shape and character requirement are looked concrete purposes and are decided.Be mainly used in aircraft sensor window, reconnaissance plane investigation window, vehicle window and guided missile dome etc.Along with the further developing of infrared window, requirements at the higher level have been proposed material of infrared window in recent years, except that visible~in have the high permeability in the infrared wide band, also need material to have anti-EMI (electromagnetic shielding) performance.
The solution of infrared window radar invisible and anti-EMI mainly is the conductive metal mesh grid that periodic array is arranged at window surface or internal production.The investigator makes the conductive metal mesh grid (FSS) with periodic array through photoetching technique (sensitization plated film-Feng etching) on the surface of infrared window mostly both at home and abroad at present.But; Also there is very big difficulty in the metallic mesh that on big area or spherical substrate, is coated with sensitization-lithographic technique making hachure; Simultaneously the thermal conductivity coefficient of metallic mesh and infrared sill differs greatly, and the actual related fields such as firmness, heat shock resistance, resisting laser damage that are coated on thickness on the infrared sill and are the metallic mesh film of submicron order remain very big challenge.Institute of United States Navy is at (S.S.Bayya et.al.VIS-IR transmitting windows.SPIE5786 (2005): 262-271) announce a kind of specified shape method wiry that between infrared glass and another kind of infra-red material, adds in the international conference; Through with glass heats to more than the softening temperature; Glass and another kind of infra-red material bonding obtain a kind of compound infrared window with anti-EMI.This method has advantages such as advantages of good shielding performance, thermal shock resistance be good.But in article, do not announce detailed glass composition.USP (Low loss visible-IR transmitting glass-al μ min μ m oxynitride composites and process Patent Application No.: 7927705 (2007)) announced the technical scheme of a kind of bismuth germanate glass and ALON infra-red china composition metal grid, embodied good shield effectiveness.Because this transition temperature of forming glass is high, and in the heating recombination process, glass is prone to surperficial crystallization, makes large-sized composite material prepare difficulty.
Chinese patent patent No. ZL200610028867: pass through visible with in infrared germanium gallate glass) in; Announced a kind of good infrared glass composition; But in the elevated temperature heat recombination process; Be prone to surperficial crystallization,, have a strong impact on infrared transmission performance at two kinds of opaque interfaces of infra-red material intermediate formation.
Summary of the invention
The purpose of this invention is to provide a kind of infrared window glass; To overcome infrared glass at high temperature (more than the transition temperature; Crystallization begins below the temperature) surperficial crystallization phenomenon in the heat treatment process; Compound infra-red material is in defective such as bubble, impure point at the interface, and formation composite windows such as this infrared window glass and germanate infrared glass, white gem crystal have very high transmitance in middle-infrared band (3~5 μ m).
The basic ideas that the present invention forms adjustment to glass are: on the basis of the germanium gallate composition with fine glass formation ability; Through introducing the part alkalimetal oxide; Further improve the anti-crystallization property of glass, especially effectively suppressed glass surface and formed Ba
2GeO
4Crystalline trend has reduced the glass characteristic temperature simultaneously.Adopt the glass of composition of the present invention preparation, through after adding wire cloth in the middle of two blocks of glass, more than glass transformation temperature 20 ℃; Crystallization begins below the temperature; Long-time heat preservation sintering under the vacuum obtains a kind of multi-functional composite window material: glass does not have obviously visible interface, and wire cloth distributes wherein; Composite sample has good anti-electromagnetic interference performance, has very high transmitance at 3~5 mu m wavebands simultaneously.
Technical solution of the present invention is following:
A kind of visible with in infrared germanium gallate glass, the composition and the molar percentage thereof of this glass are following:
Wherein: M is one or more among Ba, Ca, the Sr, and its content sum is between 30~45mol%; N is one or more among Na, K, the Cs, and its content sum is between 5~15mol%.
Infrared glass preparation method of the present invention comprises technological processs such as taking conventional high temperature melting fusing, cast, annealing, and wherein the fusion stage is taked the protection of liquid carbon dioxide gasifying gas, and annealing process is taked to carry out under the liquid nitrogen protection.
The Composite Preparation process of described glass and glass or white gem crystal comprises; Two kinds of infra-red material compound one sides all are polished to more than the requirement of minimum opticglass opposite type, smooth finish; Polished surface is corresponding; Last held (adding wire cloth perhaps) in high-temperature vacuum furnace, is evacuated to 10
-4More than the handkerchief, more than glass transformation temperature 20 ℃, crystallization begins below the temperature, and soaking time slowly cooled to room temperature greater than 36 hours, obtain the not having visible interface high transparent sample of (or accompanying metal grill).
Technique effect of the present invention is following:
This infrared window glass is particularly suitable for forming composite window with germanate infrared glass, white gem crystal etc., and the compound interface of two kinds of infra-red materials does not have defectives such as bubble, crystallization, and infrared transmittivity is high.Can overcome the surperficial crystallization phenomenon of existing infrared glass in high temperature (more than the transition temperature, crystallization begins below the temperature) heat treatment process, compound infra-red material is in defective such as bubble, impure point at the interface,
Embodiment
Embodiment 1, adopts 25GeO of the present invention
2+ 20Ga
2O
3+ 44BaO+5Al
2O
3+ 1BaCl
2+ 5Na
2CO
3Form (mol%), under the liquefied carbon dioxide gas protection, prepare the high quality infrared glass.With two identical infrared glasses precise polished after, be stacked in up and down in the vacuum oven, 10
-4Under the high vacuum of handkerchief, slowly be warming up to 615 ℃ through 10 hours, be incubated after 20 hours, slowly be cooled to room temperature, obtain the glass/glass composite sample from room temperature.Composite sample does not have obviously visible compound interface, and the average transmittances of uncoated 6mm thickness sample in 3~5 mu m ranges is greater than 73%.
Embodiment 2, adopt 15GeO of the present invention
2+ 25Ga
2O
3+ 40BaO+8Al
2O
3+ 5BaCl
2+ 1
2Na
2CO
3Form (mol%), under the liquefied carbon dioxide gas protection, prepare the high quality infrared glass.With this infrared glass and same size white stone precise polished after, be stacked in up and down in the vacuum oven, 10
-4Under the high vacuum of handkerchief, slowly be warming up to 585 ℃ through 10 hours, be incubated after 20 hours, slowly be cooled to room temperature, obtain the compound infrared window sample of glass/white stone from room temperature.Composite sample does not have obviously visible compound interface, and the average transmittances of uncoated 6mm thickness sample in 3~5 mu m ranges is greater than 70%.
The composition of the embodiment 3,4,5,6,7,8,9 of infrared window glass of the present invention is as shown in the table, takes the 2 similar technologies with embodiment, the compound infrared window that obtains having high-clarity, and its transmitance is greater than 70%.
GeO 2 | Ga 2O 3 | BaO | CaO | SrO | Al 2O 3 | BaCl 2 | Na 2CO 3 | K 2CO 3 | Cs 2CO 3 | |
3 | 16 | 24 | 30 | 5 | 5 | 8 | 5 | 12 | ||
4 | 16 | 24 | 40 | 8 | 5 | 12 | ||||
5 | 16 | 24 | 40 | 8 | 5 | 12 | ||||
6 | 16 | 24 | 20 | 20 | 8 | 5 | 6 | 6 | ||
7 | 16 | 24 | 20 | 10 | 10 | 8 | 5 | 6 | 6 | |
8 | 16 | 24 | 15 | 25 | 8 | 5 | 6 | 6 | ||
9 | 16 | 24 | 10 | 30 | 8 | 5 | 4 | 4 | 4 |
Annotate: because MO is among BaO, CaO, the SrO one or more in composition, its glass property is similar, to compound effect also all fours, no longer carries out exhaustive for the embodiment of its different permutation and combination; Same N
2CO
3Be Na
2CO
3, K
2CO
3, Cs
2CO
3In one or more, its glass property is similar, to compound effect also all fours, no longer carries out exhaustive for the embodiment of its different permutation and combination.
Embodiment 10, adopt 21GeO of the present invention
2+ 15Ga
2O
3+ 45BaO+10Al
2O
3+ 2BaCl
2+ 7K
2CO
3Form (mol%), under the liquefied carbon dioxide gas protection, prepare the high quality infrared glass.With two identical infrared glasses precise polished after, sandwich the specified shape grid of same size between the glass, be stacked in up and down in the vacuum oven, 10
-4Under the high vacuum of handkerchief, slowly be warming up to 603 ℃ through 10 hours, be incubated after 20 hours, slowly be cooled to room temperature, obtain glass/metal screen grid/glass composite sample from room temperature.Composite sample does not have obviously visible compound interface, and the average transmittances of uncoated 6mm thickness sample in 3~5 mu m ranges is greater than 63%, to the electromagnetic shield effectiveness that shows average-22db of 10~18GHz.
Embodiment 11, adopt 24GeO of the present invention
2+ 22Ga
2O
3+ 30BaO+5Al
2O
3+ 4BaCl
2+ 15Na
2CO
3Form (mol%), under the liquefied carbon dioxide gas protection, prepare the high quality infrared glass.With infrared glass and same size white stone precise polished after, sandwich the specified shape grid of same size between glass and the jewel, be stacked in up and down in the vacuum oven, 10
-4Under the high vacuum of handkerchief, slowly be warming up to 598 ℃ through 10 hours, be incubated after 20 hours, slowly be cooled to room temperature, obtain glass/metal screen grid/white stone composite sample from room temperature.Composite sample does not have obviously visible compound interface, and the average transmittances of uncoated 6mm thickness sample in 3~5 mu m ranges is greater than 55%, to the electromagnetic shield effectiveness that shows average-21db of 10~18GHz.
Embodiment 12, adopt 20GeO of the present invention
2+ 20Ga
2O
3+ 20BaO+18CaO+8Al
2O
3+ 2BaCl
2+ 12Cs
2CO
3Form (mol%), under the liquefied carbon dioxide gas protection, prepare the high quality infrared glass.With infrared glass and same size white stone precise polished after, sandwich the specified shape grid of same size between glass and the jewel, be stacked in up and down in the vacuum oven, 10
-4Under the high vacuum of handkerchief, slowly be warming up to 605 ℃ through 10 hours, be incubated after 20 hours, slowly be cooled to room temperature, obtain glass/metal screen grid/white stone composite sample from room temperature.Composite sample does not have obviously visible compound interface, and the average transmittances of uncoated 6mm thickness sample in 3~5 mu m ranges is greater than 55%, to the electromagnetic shield effectiveness that shows average-22db of 10~18GHz.
Embodiment 13, adopt 17GeO of the present invention
2+ 23Ga
2O
3+ 20BaO+10CaO+10SrO+7Al
2O
3+ 3BaCl
2+ 10Cs
2CO
3Form (mol%), under the liquefied carbon dioxide gas protection, prepare the high quality infrared glass.With infrared glass and same size white stone precise polished after, sandwich the specified shape grid of same size between glass and the jewel, be stacked in up and down in the vacuum oven, 10
-4Under the high vacuum of handkerchief, slowly be warming up to 612 ℃ through 10 hours, be incubated after 20 hours, slowly be cooled to room temperature, obtain glass/metal screen grid/white stone composite sample from room temperature.Composite sample does not have obviously visible compound interface, and the average transmittances of uncoated 6mm thickness sample in 3~5 mu m ranges is greater than 55%, to the electromagnetic shield effectiveness that shows average-23db of 10~18GHz.
Claims (1)
Priority Applications (1)
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CN2011102646240A CN102432174A (en) | 2011-09-08 | 2011-09-08 | Infrared window glass |
Applications Claiming Priority (1)
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CN2011102646240A CN102432174A (en) | 2011-09-08 | 2011-09-08 | Infrared window glass |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103442544A (en) * | 2013-08-28 | 2013-12-11 | 中国科学院上海光学精密机械研究所 | Manufacturing method for electromagnetic shielding light window of internally-embedded type woven-wire fence |
CN104749735A (en) * | 2015-03-31 | 2015-07-01 | 中国科学院长春光学精密机械与物理研究所 | Splicing type conformal optical window |
CN111148387A (en) * | 2019-12-13 | 2020-05-12 | 武汉航空仪表有限责任公司 | Electromechanical controller observation window |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1884166A (en) * | 2006-07-12 | 2006-12-27 | 中国科学院上海光学精密机械研究所 | Visible and mid-infrared transparent germanate gallate glass |
CN101172776A (en) * | 2007-10-30 | 2008-05-07 | 上海应用技术学院 | Infrared transparent rare earth-containing germanate glass and method of manufacturing the same |
CN101182118A (en) * | 2007-11-23 | 2008-05-21 | 暨南大学 | Alkali metal lanthanum bismuthate gallate infrared optical glass and method for making same |
CN101184700A (en) * | 2005-04-28 | 2008-05-21 | 株式会社小原 | Optical glass |
WO2008075546A1 (en) * | 2006-12-19 | 2008-06-26 | Asahi Glass Company, Limited | Glass for substrate |
-
2011
- 2011-09-08 CN CN2011102646240A patent/CN102432174A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101184700A (en) * | 2005-04-28 | 2008-05-21 | 株式会社小原 | Optical glass |
CN1884166A (en) * | 2006-07-12 | 2006-12-27 | 中国科学院上海光学精密机械研究所 | Visible and mid-infrared transparent germanate gallate glass |
WO2008075546A1 (en) * | 2006-12-19 | 2008-06-26 | Asahi Glass Company, Limited | Glass for substrate |
CN101172776A (en) * | 2007-10-30 | 2008-05-07 | 上海应用技术学院 | Infrared transparent rare earth-containing germanate glass and method of manufacturing the same |
CN101182118A (en) * | 2007-11-23 | 2008-05-21 | 暨南大学 | Alkali metal lanthanum bismuthate gallate infrared optical glass and method for making same |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103442544A (en) * | 2013-08-28 | 2013-12-11 | 中国科学院上海光学精密机械研究所 | Manufacturing method for electromagnetic shielding light window of internally-embedded type woven-wire fence |
CN103442544B (en) * | 2013-08-28 | 2016-08-10 | 中国科学院上海光学精密机械研究所 | The preparation method of the electromagnetic shielding optical window of embedded metal grid |
CN104749735A (en) * | 2015-03-31 | 2015-07-01 | 中国科学院长春光学精密机械与物理研究所 | Splicing type conformal optical window |
CN111148387A (en) * | 2019-12-13 | 2020-05-12 | 武汉航空仪表有限责任公司 | Electromechanical controller observation window |
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Application publication date: 20120502 |