CN107021622A - A kind of infrared glass preparation method and its de-watering apparatus - Google Patents
A kind of infrared glass preparation method and its de-watering apparatus Download PDFInfo
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- CN107021622A CN107021622A CN201710197410.3A CN201710197410A CN107021622A CN 107021622 A CN107021622 A CN 107021622A CN 201710197410 A CN201710197410 A CN 201710197410A CN 107021622 A CN107021622 A CN 107021622A
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- infrared
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- 239000011521 glass Substances 0.000 title claims abstract description 77
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000460 chlorine Substances 0.000 claims abstract description 38
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 38
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000011261 inert gas Substances 0.000 claims abstract description 34
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000007789 gas Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims description 11
- 239000010453 quartz Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 229910052717 sulfur Inorganic materials 0.000 claims description 7
- 239000003708 ampul Substances 0.000 claims description 6
- 238000010791 quenching Methods 0.000 claims description 6
- 235000019353 potassium silicate Nutrition 0.000 claims description 5
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052787 antimony Inorganic materials 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229910052785 arsenic Inorganic materials 0.000 claims description 4
- 229910052733 gallium Inorganic materials 0.000 claims description 4
- 229910052732 germanium Inorganic materials 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 230000000171 quenching effect Effects 0.000 claims description 4
- 229910003069 TeO2 Inorganic materials 0.000 claims description 3
- 230000004927 fusion Effects 0.000 claims description 3
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 claims description 3
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000002242 deionisation method Methods 0.000 claims 1
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 238000007781 pre-processing Methods 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 10
- 239000001257 hydrogen Substances 0.000 abstract description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000156 glass melt Substances 0.000 abstract description 6
- 239000001301 oxygen Substances 0.000 abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 abstract description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 2
- 239000007800 oxidant agent Substances 0.000 abstract description 2
- 238000010792 warming Methods 0.000 description 11
- 238000010521 absorption reaction Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 229910052958 orpiment Inorganic materials 0.000 description 5
- 239000005387 chalcogenide glass Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910001428 transition metal ion Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229940123973 Oxygen scavenger Drugs 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 238000003331 infrared imaging Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 230000004297 night vision Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- XHGGEBRKUWZHEK-UHFFFAOYSA-L tellurate Chemical compound [O-][Te]([O-])(=O)=O XHGGEBRKUWZHEK-UHFFFAOYSA-L 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- 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
- C03C3/12—Silica-free oxide glass compositions
- C03C3/122—Silica-free oxide glass compositions containing oxides of As, Sb, Bi, Mo, W, V, Te as glass formers
-
- 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
- C03C3/32—Non-oxide glass compositions, e.g. binary or ternary halides, sulfides or nitrides of germanium, selenium or tellurium
- C03C3/321—Chalcogenide glasses, e.g. containing S, Se, Te
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B7/00—Drying solid materials or objects by processes using a combination of processes not covered by a single one of groups F26B3/00 and F26B5/00
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Glass Compositions (AREA)
Abstract
The invention belongs to glasses for infrared use preparation field, and in particular to a kind of infrared glass preparation method and its de-watering apparatus, to solve to be difficult in the prior art effectively to remove the hydrogen in infrared glass, oxygen impurities defect.Including inert gas inleting pipe, chlorine air inlet pipe, heating furnace, mother tube and escape pipe, the inert gas inleting pipe, chlorine air inlet pipe and escape pipe are connected with mother tube respectively, and heating furnace is arranged on outside the mother tube.Infrared glass is removed water using chlorine, the absworption peak produced in infrared glass by O H and H S keys at 2.9 and 4.3 microns can be effectively removed, is that the practical of infrared glass lays the foundation.The technical principle mainly uses strong oxidizer chlorine to grab the hydrogen impurity in glass, and generates in hydrogen chloride gas discharge glass melts, so as to eliminate hydrogen impurity.
Description
Technical field
The invention belongs to glasses for infrared use preparation field, and in particular to a kind of infrared glass preparation method and its water removal dress
Put.
Background technology
Glasses for infrared use have weight in fields such as modern national defense, space exploration, mid and far infrared light source and infrared imagings
The application value wanted.It is all too busy to get away red that guidance, infrared early warning, the observation of such as various guided missiles aim at high energy beam interception weapon etc.
Outer window material；High score earth observation systems service band includes middle-infrared band, it is also desirable to made using glasses for infrared use
Its infrared window；On civilian, the infrared night vision system of infrared viewing device and high-grade car assembling all needs glasses for infrared use to do
Eyes.
The limitation wide variety of main bottleneck of infrared glass is that infrared glass impurity is more at present, and purity is inadequate.Infrared glass
Glass is very sensitive to impurity, and micro carbon, hydrogen, the presence of oxygen and transition metal ions will produce serious infrared absorption.Arrive
So far, it can be very good to control transition metal ion content by using high pure raw material, eliminate the miscellaneous of transition metal generation
Infrared absorption.But because the presence containing oxygen and vapor in air, current preparation technology is still difficult to effective suppression
Hydrogen manufacturing and the infrared absorption of oxygen impurities.
Publication No. 103319070B Chinese patent (publication date is 2015-12-09), although improve chalcogenide glass
Infrared absorption, but still have obvious Impurity Absorption peak in 3~5 micron wavebands.Publication No. 102531335A China
(publication date is 2013-02- to patent (publication date is 2012-07-04) and Publication No. 102936090A Chinese patent
20) method of purification proposed is primarily directed to eliminate oxygen impurities, it is difficult to effectively remove dehydrogenation impurity.And oxygen scavenger used
Aluminium or magnesium and reaction of Salmon-Saxl, therefore it is not suitable for the chalcogenide glass of sulfur-bearing.
The content of the invention
The purpose of the present invention is：A kind of infrared glass preparation method and its de-watering apparatus are provided, to solve prior art
In be difficult to effectively remove infrared glass in hydrogen, the defect of oxygen impurities.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of infrared glass preparation method, it is characterized in that：Comprise the following steps：
1) glass preparation raw material, fusion cast glass clinker are weighed；
2) the glass clinker is placed in the mother tube by pretreatment, is passed through inert gas 30~120 minutes；
3) flow of inert gas is kept, the mother tube is heated to 450~900 DEG C, then be passed through 30~120 points of chlorine
Clock；
4) flow of inert gas is kept, stopping is passed through chlorine, stops heating, is cooled to room temperature, obtains except waterglass is ripe
Material；
5) required infrared glass is obtained after being annealed through quenching except waterglass clinker is melted again by described.
Further, the step 2) in, the method that implements of the pretreatment is：Mother tube 10 is cleaned with ultrasonic wave
Minute, soaked 5 minutes with chloroazotic acid afterwards, then deionized water rinsed clean is used, it is placed in vacuum drying oven, 3 is incubated at 1000 DEG C small
When, it is slowly dropped to room temperature.
Further, the inert gas is nitrogen or argon gas or helium.
Further, the flow of the inert gas is 30~100ml/min.
Further, the flow of the chlorine is 3~10ml/min.
Further, the raw material is As and S or Ge, Ga, Sb and S or TeO2, BaO and ZnO.
The present invention is also provided based on a kind of above-mentioned de-watering apparatus of infrared glass preparation method, and it is characterized in that：Bag
Include inert gas inleting pipe, chlorine air inlet pipe, heating furnace, mother tube and escape pipe, the inert gas inleting pipe, chlorine air inlet
Pipe and escape pipe are connected with mother tube respectively, and heating furnace is arranged on outside the mother tube.
Further, the inert gas inleting pipe, chlorine air inlet pipe, mother tube and escape pipe are quartz ampoules.
Further, the hydroxy radical content of the quartz ampoule is less than 10ppm.
The present invention is relative to the beneficial effect of prior art：Infrared glass is removed water using chlorine, can effectively be removed
The absworption peak produced in infrared glass by O-H and H-S keys at 2.9 and 4.3 microns is removed, is that the practical of infrared glass establishes base
Plinth.The technical principle mainly uses strong oxidizer chlorine to grab the hydrogen impurity in glass, and generates hydrogen chloride gas discharge
In glass melts, so as to eliminate hydrogen impurity.Its reactional equation is：[O-H-]+S2-→[H-S]+O2-[H-S]+Cl2→HCl↑+S2-
Brief description of the drawings
Fig. 1 is the structural representation of de-watering apparatus in the present invention；
Fig. 2 is high-purity As prepared by the present invention2S3The As that glass is prepared with prior art2S3The mid and far infrared of glass is passed through
Spectrum comparison diagram；
Fig. 3 is high-purity Ge prepared by the present invention20Ga5Sb10S65The Ge that glass is prepared with prior art20Ga5Sb10S65Glass
Mid and far infrared pass through spectrum comparison diagram；
Fig. 4 is high-purity 60TeO prepared by the present invention2The 60TeO that -20BaO -20ZnO glass is prepared with prior art2–
The mid and far infrared of 20BaO -20ZnO glass passes through spectrum comparison diagram；
In figure, 1- inert gas inleting pipes, 2- chlorine air inlet pipe, 3- heating furnaces, 4- mother tubes, 5- escape pipes.
Embodiment
The present invention is described further with reference to specific embodiments and the drawings.
As shown in figure 1, the invention provides a kind of de-watering apparatus for preparing high-purity infrared glass, including inert gas air inlet
Pipe 1, chlorine air inlet pipe 2, heating furnace 3, mother tube 4 and escape pipe 5, wherein, inert gas inleting pipe 1 is located at the one of mother tube 4
Side and be connected with mother tube 4, chlorine air inlet pipe 2 is located on mother tube 4 and is connected with mother tube, escape pipe 5 is arranged on original
The opposite side of expects pipe is simultaneously connected with mother tube 4, and heating furnace 3 is arranged on outside mother tube 4.Air inlet pipe 1, chlorine air inlet pipe 2, original
Expects pipe 4 and escape pipe 5 are quartz ampoules.Quartz ampoule be hydroxy radical content be less than 10ppm clean quartz ampoule, quartz ampoule have passed through as
Lower processing：It is less than 10ppm quartz ampoule from hydroxy radical content, is cleaned 10 minutes, soaked 5 minutes with chloroazotic acid afterwards with ultrasonic wave,
Deionized water rinsed clean is used again, is placed in vacuum drying oven, is incubated 3 hours at 1000 DEG C, is slowly dropped to room temperature.
Technical process comprises the following steps：
1) frit is weighed according to formula, 500~1000 DEG C of fusion cast glass clinkers is warming up to by traditional melting technology；
2) glass clinker is placed in mother tube 4, inert gas inleting pipe 1 and chlorine air inlet pipe 2 is respectively connected to inertia
Gas piping and chlorine pipeline, first lead to inert gas 30-120 minutes；
3) keep inert gas flow certain, open heating furnace 3, be warming up to 450-900 DEG C, open chlorine, the time is in 30-
Between 120 minutes；
4) keep inert gas flow certain, stop logical chlorine, stop heating, treat that mother tube 4 is cooled to room temperature, removed
Waterglass clinker；
5) the glass clinker by water removal is warming up into 500~1000 DEG C by traditional melting technology to melt again, founded
Cheng Hou, glass melts obtain final high-purity infrared glass after being annealed through quenching.
Can select raw material is As and S, and obtained infrared glass component is As2S3, or raw material be Ge, Ga, Sb and S, it is obtained
Infrared glass component is Ge20Ga5Sb10S65, or raw material is TeO2, BaO and ZnO, obtained infrared glass component is 60TeO2–
20BaO–20ZnO。
Illustrate with reference to embodiments：
Embodiment one：Using component as As2S3High-purity chalcogenide glass preparation exemplified by, comprise the following specific steps that：
1) according to As2S3Formula weighs the sulphur and arsenic simple substance raw material that purity is 99.999%, is warming up to traditional rocking furnace
800 DEG C, found 12 hours, obtain glass clinker；
2) by As2S3Glass clinker is placed in mother tube 4, and inert gas inleting pipe 1 and chlorine air inlet pipe 2 are respectively connected to
Nitrogen pipeline and chlorine pipeline, first lead to nitrogen, and flow is 30ml/min, and the time is 120 minutes；
3) inert gas flow is kept, heating furnace 3 is opened, is warming up to 500 DEG C, opens chlorine, flow is 10ml/min, when
Between be 40 minutes；
4) inert gas flow is kept, stops logical chlorine, stops heating, treat that mother tube 4 is cooled to room temperature, removed water
As2S3Glass clinker；
5) by the As by water removal2S3Glass clinker is warming up to 800 DEG C by traditional melting technology, founds again 3 hours, melts
After the completion of system, glass melts obtain final high-purity As after being annealed through quenching2S3Infrared glass.
Fig. 2 is high-purity As prepared by above-described embodiment2S3The As that glass is prepared with prior art2S3The mid and far infrared of glass
Through 5 millimeters of spectrum comparison diagram test sample thickness.Prove that this method can effectively eliminate the miscellaneous of middle-infrared band by contrasting
Matter absorbs.
Embodiment two：Using component as Ge20Ga5Sb10S65High-purity chalcogenide glass preparation exemplified by, comprise the following specific steps that：
1) according to Ge20Ga5Sb10S65Formula weighs germanium, gallium, antimony and the sulphur simple substance raw material that purity is 99.999%, with tradition
Rocking furnace is warming up to 950 DEG C, founds 12 hours, obtains glass clinker；
2) by Ge20Ga5Sb10S65Glass clinker is placed in mother tube 4, by inert gas inleting pipe 1 and chlorine air inlet pipe 2
Argon gas and chlorine pipeline are respectively connected to, first leads to argon gas, flow is 80ml/min, and the time is 30 minutes；
3) inert gas flow is kept, heating furnace 3 is opened, is warming up to 650 DEG C, opens chlorine, flow is 4ml/min, when
Between be 100 minutes；
4) inert gas flow is kept, stops logical chlorine, stops heating, treat that mother tube 4 is cooled to room temperature, removed water
Ge20Ga5Sb10S65Glass clinker；
5) by the Ge by water removal20Ga5Sb10S65Glass clinker is warming up to 950 DEG C by traditional melting technology, and 6 are founded again
Hour, after the completion of founding, glass melts obtain final high-purity Ge after being annealed through quenching20Ga5Sb10S65Infrared glass.
Fig. 3 is high-purity Ge prepared by above-described embodiment20Ga5Sb10S65The Ge that glass is prepared with prior art20Ga5Sb10S65
The mid and far infrared of glass passes through 5 millimeters of spectrum comparison diagram test sample thickness.Prove that this method can be effectively eliminated by contrasting
The Impurity Absorption of middle-infrared band.
Embodiment three：Using component as 60TeO2- 20BaO -20ZnO high-purity tellurate glass is prepared as example, including as follows
Specific steps：
1) according to 60TeO2- 20BaO -20ZnO formulas weigh the TeO that purity is 99.99%2, BaO and ZnO raw materials, load
Gold crucible, is placed in Muffle furnace, is warming up to 800 DEG C, founds 2 hours, obtains glass clinker；
2) by 60TeO2- 20BaO -20ZnO glass clinkers are placed in mother tube 4, and inert gas inleting pipe 1 and chlorine are entered
Tracheae 2 is respectively connected to helium and chlorine pipeline, first helium injection gas, and flow is 50ml/min, and the time is 60 minutes；
3) inert gas flow is kept, heating furnace 3 is opened, is warming up to 700 DEG C, opens chlorine, flow is 6ml/min, when
Between be 60 minutes；
4) inert gas flow is kept, stops logical chlorine, stops heating, treat that mother tube 4 is cooled to room temperature, removed water
60TeO2- 20BaO -20ZnO glass clinkers；
5) by the 60TeO by water removal2- 20BaO -20ZnO glass clinker loads gold crucible, is placed in Muffle furnace, rises
Temperature is founded 2 hours, after the completion of founding, glass melts obtain final high-purity infrared glass after being annealed through quenching again to 800 DEG C
Glass.
Fig. 4 is high-purity 60TeO prepared by above-described embodiment2The 60TeO that -20BaO -20ZnO glass is prepared with prior art2–
The mid and far infrared of 20BaO -20ZnO glass passes through 5 millimeters of spectrum comparison diagram test sample thickness.Prove that this method can by contrasting
Effectively eliminate the Impurity Absorption of middle-infrared band.
Claims (9)
1. a kind of infrared glass preparation method, it is characterised in that：Comprise the following steps：
1) glass preparation raw material, fusion cast glass clinker are weighed；
2) the glass clinker is placed in the mother tube by pretreatment, is passed through inert gas 30~120 minutes；
3) flow of inert gas is kept, the mother tube is heated to 450~900 DEG C, then be passed through chlorine 30~120 minutes；
4) flow of inert gas is kept, stopping is passed through chlorine, stops heating, is cooled to room temperature, obtains removing waterglass clinker；
5) required infrared glass is obtained after being annealed through quenching except waterglass clinker is melted again by described.
2. a kind of infrared glass preparation method according to claim 1, it is characterised in that：The step 2) in, it is described pre-
Processing the method that implements be：Mother tube is cleaned with ultrasonic wave 10 minutes, soaked 5 minutes with chloroazotic acid afterwards, then use deionization
Water rinsed clean, is placed in vacuum drying oven, is incubated 3 hours at 1000 DEG C, is slowly dropped to room temperature.
3. a kind of infrared glass preparation method according to claim 1 or 2, it is characterised in that：The inert gas is nitrogen
Gas or argon gas or helium.
4. a kind of infrared glass preparation method according to claim 1 or 2, it is characterised in that：The stream of the inert gas
Measure as 30~100ml/min.
5. a kind of infrared glass preparation method according to claim 4, it is characterised in that：The flow of the chlorine be 3~
10ml/min。
6. a kind of infrared glass preparation method according to claim 5, it is characterised in that：The raw material be As and S or Ge,
Ga, Sb and S or TeO2, BaO and ZnO.
7. the de-watering apparatus based on a kind of infrared glass preparation method described in claim 1-6 any one, it is characterised in that：
Including inert gas inleting pipe, chlorine air inlet pipe, heating furnace, mother tube and escape pipe, the inert gas inleting pipe, chlorine enter
Tracheae and escape pipe are connected with mother tube respectively, and heating furnace is arranged on outside the mother tube.
8. de-watering apparatus according to claim 7, it is characterised in that：The inert gas inleting pipe, chlorine air inlet pipe, original
Expects pipe and escape pipe are quartz ampoules.
9. de-watering apparatus according to claim 8, it is characterised in that：The hydroxy radical content of the quartz ampoule is less than 10ppm.
Priority Applications (1)
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| CN201710197410.3A CN107021622A (en) | 2017-03-29 | 2017-03-29 | A kind of infrared glass preparation method and its de-watering apparatus |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710197410.3A CN107021622A (en) | 2017-03-29 | 2017-03-29 | A kind of infrared glass preparation method and its de-watering apparatus |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108275875A (en) * | 2018-02-01 | 2018-07-13 | 中国建筑材料科学研究总院有限公司 | Vulcanize zinc modification chalcogenide glass and preparation method thereof |
| CN111253058A (en) * | 2020-01-22 | 2020-06-09 | 中国科学院西安光学精密机械研究所 | Device and method for preparing anhydrous infrared glass optical fiber preform |
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| CN108275875A (en) * | 2018-02-01 | 2018-07-13 | 中国建筑材料科学研究总院有限公司 | Vulcanize zinc modification chalcogenide glass and preparation method thereof |
| CN111253058A (en) * | 2020-01-22 | 2020-06-09 | 中国科学院西安光学精密机械研究所 | Device and method for preparing anhydrous infrared glass optical fiber preform |
| CN111253058B (en) * | 2020-01-22 | 2021-09-14 | 中国科学院西安光学精密机械研究所 | Device and method for preparing anhydrous infrared glass optical fiber preform |
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