CN103332851A - Preparation method of high-purity and low-loss chalcogenide glass - Google Patents
Preparation method of high-purity and low-loss chalcogenide glass Download PDFInfo
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- CN103332851A CN103332851A CN2013102196093A CN201310219609A CN103332851A CN 103332851 A CN103332851 A CN 103332851A CN 2013102196093 A CN2013102196093 A CN 2013102196093A CN 201310219609 A CN201310219609 A CN 201310219609A CN 103332851 A CN103332851 A CN 103332851A
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Abstract
The invention provides a preparation method of high-purity and low-loss chalcogenide glass, belonging to a preparation method of the chalcogenide glass. The preparation method comprises the following steps of: removing hydrocarbon impurity in the glass by taking ultra-dry gallium chloride as a purifying agent, and distilling and purifying the glass in combination with the conventional deoxidant, aluminum, magnesium or zirconium metal; placing glass mixture into a quartz ampoule to be sealed in by means of vacuum supply, founding the glass mixture in a vacuum ampoule, dynamically distilling the glass, and remelting the mixture after distilling; and effectively removing the hydrocarbon impurity in the glass by taking the ultra-dry gallium chloride as the purifying agent, so that the Mie scattering imperfection is hardly formed in the finally-obtained high-purity chalcogenide glass, and the low-loss homogeneous glass can be obtained. According to the high-purity chalcogenide glass synthesized by the preparation method provided by the invention, the minimum loss under the infrared transmission waveband is less than 0.3dB/m, and the corresponding loss of the absorption peak of the residual impurity is less than 8dB/m, so that the preparation method can be used in the field of an infrared glass optical element and an infrared optical fiber. The ultra-dry gallium chloride purifying agent can be easily obtained, and is lower in price; the carbon, hydrogen and oxygen impurities can be removed from the chalcogenide glass at high efficiency; the prepared chalcogenide glass is better in uniformity and less in light scattering.
Description
Technical field
The present invention relates to a kind of preparation method of chalcogenide glass, particularly a kind of preparation method of high-purity low-loss chalcogenide glass.
Background technology
Chalcogenide glass refers to that with periodictable VIA family element S, Se, Te be the main amorphous material of introducing a certain amount of other metal or non-metallic element formation.Because higher atomic mass and more weak chemical bond are strong, chalcogenide glass has lower vibration phonon energy, thereby makes them have excellent transmission performance at infrared band.In chalcogenide glass, the typical transmission range of sulfide, selenide and tellurite glass is respectively 0.5-10 μ m, 0.8-14 μ m, 1.5-20 μ m.Have extremely important application background and potentiality by the infrared optical element of chalcogenide glass making and the optical fiber of drawing in thermal imaging, infrared laser transmission, chemistry and fields such as bio-sensing, outer space detection.
Although chalcogenide glass adopts high pure raw material to found under vacuum environment usually, the surface of raw material, the inwall of quartz ampoule, experimental situation etc. tend to introduce impurity such as a certain amount of carbon, hydrogen, oxygen, these impurity have strong absorption at 1-15 μ m, and make easily in the glass and to form micro-bubble or micron-sized heterogeneous inclusion, infrared light transmission performance to glass produces serious negative impact, even causes chalcogenide glass optical element or optical fiber to use.Therefore, obtaining the low-loss chalcogenide glass of high purity is preparation relevant optical and the basis that draws low loss fiber and crucial.
High-purity chalcogenide glass adopts usually to prepare under the purification reaction atmosphere or pass through to add the laggard oozy glass distillation of purifying agent and obtains.The former complicated operation, safety precautions is had relatively high expectations, and glass ingredient is difficult for accurately control; Latter's operation is simple relatively, and glass distillation front and back composition changes less, and purification process is easier to control.At present, distillation glass was effectively removed after oxygen impurities in the chalcogenide glass adopted usually and adds aluminium, magnesium or zirconium metal oxygen scavenger, the resultant of reaction of oxygen impurities has extremely low vapour pressure in distillation temperature in oxygen scavenger and the glass, and this resultant of reaction can remain in the still tube in the process of distillation glass.For the C in the glass and H impurity, adopt usually to add the dried AlCl of the excess of imports
3Perhaps TeCl
4Distillation glass is effectively removed behind the purifying agent.The resultant of reaction CCl of purifying agent and C and H impurity
4Having very high vapour pressure with HCl in distillation temperature, can be taken away in the dynamic still-process of glass open formula, and the chalcogenide glass with moderate vapour pressure can liquefy and be set in the cold junction of still tube in still-process.Yet, when with AlCl
3During for purifying agent, the aluminum contained compound that reaction generates is or/and have neither part nor lot in the AlCl of reaction
3Easily part enters in the glass after the distillation, tends to form heterogeneous inclusion in the final glass that obtains, and causes the Mie scattering, influences the infrared light transmission performance of glass.TeCl
4There are not the problems referred to above, because Te itself is exactly sulfur family element, are soluble in chalcogenide glass, but super dried TeCl
4Be difficult to obtain.Therefore, the easy agent of glassivation efficiently that obtains of searching is most important to high-purity low-loss chalcogenide glass that preparation has high uniformity.
Summary of the invention
The objective of the invention is to, a kind of method for preparing high-purity low-loss chalcogenide glass is provided, solve the traditional preparation process method is easily introduced the heterogeneous inclusion of micron order in glass problem.
The object of the present invention is achieved like this: the preparation method introduces the super dried gallium chloride of 200-2000ppm mol ratio as the purifying agent of dehydrogenation and carbon impurity in the chalcogenide glass system, introduce aluminium, magnesium or the zirconium of 100-500ppm mol ratio as oxygen scavenger, method by dynamic distillation is purified, and obtains uniform high-purity chalcogenide glass; Concrete steps are as follows:
1, the preparation of glass compound
Form proportioning formulate glass compound in the district with the simple substance element of purity 〉=99.999% by corresponding glass, add glassivation agent and the 100-500ppm oxygen scavenger of 200-2000ppm; Blending process carries out in the inert environments of drying, and the compound hydroxy radical content of packing into is lower than in the clean quartz ampoule of 1ppm;
2, vacuumize sealing-in
To vacuumize vacuum tightness in ampoule≤10 by the quartz ampoule that step 1 gained fills compound
– 3During Pa, ampoule is placed on 100-150
oBaking is 1-4 hour in the tube furnace of C, uses oxyhydrogen flame sealing-in ampoule then;
3, glass smelting
To be put into by the good quartz ampoule that the glass compound is housed of step 2 gained sealing-in and wave stove, slowly be warming up to 800 ~ 950
oC is incubated and takes out cooling after 10 ~ 20 hours, anneals near the glass transformation temperature of correspondence then 2-5 hour;
4, the distillation of glass
The distillation of glass is carried out in the open type still tube, and the open type still tube is connected to form by a kapillary by material feeding region A and discharge zone B; The ampoule that step 3 gained is filled glass is opened in the inert environments of drying, takes out glass, the material feeding region A of the open type of packing into still tube; With soft rubber ball discharge port is blocked, vacuumized from feeding mouth, when vacuum tightness≤10
– 3During Pa from feeding mouth rear end sealing-in still tube; Still tube is put into a two warm area tube furnace, take off the discharge port soft rubber ball, and from then on end vacuumizes, when vacuum tightness≤10
– 3During Pa, slowly material feeding region A is warming up to 700-800
oC also is incubated 1 hour, simultaneously discharge zone B slowly is warming up to 200-550
oC; Glass can slowly be distilled to discharge zone B from material feeding region A, and the oxide impurity of low-steam pressure can be stayed material feeding region A, high-volatile HCl, CCl
4Can be taken away from discharge port Deng impurity, the glass that vapour pressure is moderate is stayed discharge zone B; Then respectively from discharge zone rear end and discharge zone front end sealing-in silica tube, the mixture after obtaining distilling;
5, the remelting of glass
The silica tube that step 4 gained is filled distillation back mixture is put into and is waved stove, slowly is warming up to 800 ~ 950
oC is incubated and takes out cooling after 8-12 hour, anneals near the glass transformation temperature of correspondence then 2-5 hour, slowly drops to room temperature at last, namely obtains high-purity low-loss chalcogenide glass.
Described chalcogenide glass is to be the chalcogenide glass of component with the two or more elements in germanium, arsenic, antimony, sulphur, selenium and the tellurium; Described glassivation agent is super dried gallium chloride; Described oxygen scavenger is aluminium, magnesium or zirconium metal.
Raw materials used is the high pure element of purity 〉=99.999%.
The glass distillating method that adopts is the dynamic distillating method of open type.
Beneficial effect: owing to adopted such scheme, the carbon in the glass, hydrogen and oxygen impurities have obtained the high-level efficiency removal, have obtained the chalcogenide glass of ultra-high purity; Heterogeneous inclusion significantly reduces in the glass, glass significantly improving of obtaining of homogeneity; GaCl
3Meet water generation kickback, emit hydrogenchloride, also CCl is emitted in easy and carbon impurity reaction
4, and Ga and compound thereof be soluble in chalcogenide glass, can not form heterogeneous inclusion in final glass, is a kind of comparatively ideal for the purifying agent of eliminating chalcogenide glass hydrogen and carbon impurity; Aluminium, magnesium or zirconium very easily are combined generation and are had the oxide compound of extremely-low vapor pressure with oxygen, be traditional efficient oxygen scavenger.
The ultra-pure chalcogenide glass that adopts the present invention can obtain to have following index: less than 0.3dB/m, the corresponding loss of residual impurity absorption peak is less than 8dB/m in the lowest loss of infrared permeation wavelength for glass.
Advantage of the present invention is: the easy acquisition of (1) super dried gallium chloride purifying agent and price are lower; (2) adopt the present invention to eliminate the works very well of carbon in the chalcogenide glass, hydrogen, oxygen impurities; (3) can obtain better, the littler chalcogenide glass of scattering of light of homogeneity.
Description of drawings
Fig. 1 is still tube synoptic diagram of the present invention.
Fig. 2-a is with super dried gallium chloride (GaCl
3) be purifying agent, add the aluminium oxygen scavenger, Ge-As-Se chalcogenide glass photo after distillation is purified.
Fig. 2-b is the enlarged photograph in constituency among Fig. 2-a.
Fig. 3 is that thickness is the infrared transmission spectra of 5.4mm Ge-As-Se glass before and after the distillation.
Embodiment
To further specify substantive distinguishing features of the present invention and marked improvement by embodiment below, but the present invention is not limited only to the cited case.
Embodiment 1: chalcogenide glass consists of Ge
12As
24Se
64
Be raw material with the element Ge of purity 99.999% and elements A s and the Se of purity 99.9999%, according to above-mentioned chemical constitution proportioning, add 100ppm purity and be 99.999% metal A l and 1000ppm purity and be 99.999% super dried GaCl
3, oxygen and water-content all less than the glove box that is full of nitrogen of 0.1ppm in weighing and the hydroxy radical content that cleans up in advance of packing into be lower than in the quartz ampoule of 1ppm; The quartz ampoule that fills compound is vacuumized vacuum tightness in ampoule≤10
– 3During Pa, ampoule is placed on 120
oBaking is 2 hours in the tube furnace of C, uses oxyhydrogen flame sealing-in ampoule then; The quartz ampoule that the glass compound is housed that sealing-in is good is put into and is waved stove, slowly is warming up to 900
oC is incubated to take out after 10 hours and cools off in air, then 200
oC annealing 2 hours; The ampoule that fills glass after the annealing is opened in glove box, taken out glass, in the open type of packing into the still tube (see figure 1), then glass is carried out open type and dynamically distill; The silica tube that distillation back mixture is housed put into wave stove, slowly be warming up to 900
oC is incubated to take out after 12 hours and cools off in air, then 200
oC annealing 3 hours is at last with 0.5
oThe speed of C/min drops to room temperature.Become thickness to be respectively 2mm the glass cutting that finally obtains, the sheet glass of 5mm and 10mm and twin polishing adopt the micro-camera sight glass of the near infrared inside that is operated in 940nm whether to have micron-sized heterogeneous inclusion; Detect the infrared transmission spectra of above-mentioned three kinds of thickness glass sheets, adopt the cut-back method to calculate the loss of glass; Adopt X-ray energy spectrometer to detect the variation of glass purification front and back component; Adopt the specific refractory power of prism-coupled method tested glass distillation front and back; Detected result shows: glass is observed the heterogeneous inclusion of no obvious micron order under the micro-camera of 940nm near infrared, the glass good uniformity is seen Fig. 2-a and Fig. 2-b, and the minimum spacing on the scale of glass bottom is 200 microns; The final highly pure glass that obtains is 0.25dB/m in the lowest loss of infrared permeation wave band, residual impurity absorption peak (Se-H, 4.53 μ m) corresponding loss is 7.8dB/m, sees Fig. 3, shows that carbon, hydrogen and the oxygen impurities in the glass of distillation purification back obtained efficient elimination; Form before and after the glass distillation and be respectively Ge
12.1As
23.8Se
64.1And Ge
12As
24.1Se
63.9, show that glass distillation front and back composition changes minimum; Specific refractory power at 1.55 mum wavelengths before and after the glass distillation is respectively 2.6407 ± 0.005, and 2.6415 ± 0.0002, show that glass distillation front and back specific refractory power difference is minimum.
Embodiment 2: chalcogenide glass consists of As
40S
60
Elements A s and S with purity 99.9999% are raw material, according to above-mentioned chemical constitution proportioning, add 200ppm purity and be 99.999% metal M g and 1500ppm purity and be 99.999% super dried GaCl
3, oxygen and water-content all less than the glove box that is full of nitrogen of 0.1ppm in the weighing hydroxy radical content that cleans up in advance of packing into be lower than in the quartz ampoule of 1ppm; The quartz ampoule that fills compound is vacuumized vacuum tightness in ampoule≤10
– 3During Pa, ampoule is placed on 100
oBaking is 3 hours in the tube furnace of C, uses oxyhydrogen flame sealing-in ampoule then; The quartz ampoule that the glass compound is housed that sealing-in is good is put into and is waved stove, slowly is warming up to 850
oC is incubated to take out after 15 hours and cools off in air, then 190
oC annealing 3 hours; The ampoule that fills glass after the annealing is opened in glove box, taken out glass, in the open type of packing into the still tube, then glass is carried out open type and dynamically distill; The silica tube that distillation back mixture is housed put into wave stove, slowly be warming up to 850
oC is incubated to take out after 10 hours and cools off in air, then 190
oC annealing 4 hours is at last with 0.4
oThe speed of C/min drops to room temperature.Become thickness to be respectively 2mm the glass cutting that finally obtains, the sheet glass of 5mm and 10mm and twin polishing adopt the micro-camera sight glass of the near infrared inside that is operated in 940nm whether to have micron-sized heterogeneous inclusion; Detect the infrared transmission spectra of above-mentioned three kinds of thickness glass sheets, adopt the cut-back method to calculate the loss of glass; Adopt X-ray energy spectrometer to detect the variation of glass purification front and back component; Adopt the specific refractory power of prism-coupled method tested glass distillation front and back; Detected result shows: glass is observed the heterogeneous inclusion of no obvious micron order under the micro-camera of 940nm near infrared; The final highly pure glass that obtains is 0.2dB/m in the lowest loss of infrared permeation wave band, and the corresponding loss of residual impurity absorption peak (S-H, 4.02 μ m) is 5.2dB/m; Form before and after the glass distillation and be respectively As
39.6S
60.4And As
39.8S
60.2Specific refractory power at 1.55 mum wavelengths before and after the glass distillation is respectively 2.4210 ± 0.004,2.4215 ± 0.0003.
Embodiment 3: chalcogenide glass consists of Te
20As
30Se
50
With the elements A s of purity 99.9999%, Te and Se are raw material, according to above-mentioned chemical constitution proportioning, add 150ppm purity and be 99.999% metallic Z r and 500ppm purity and be 99.999% super dried GaCl
3Oxygen and water-content all less than the glove box that is full of nitrogen of 0.1ppm in the weighing hydroxy radical content that cleans up in advance of packing into be lower than in the quartz ampoule of 1ppm; The quartz ampoule that fills compound is vacuumized vacuum tightness in ampoule≤10
– 3During Pa, ampoule is placed on 150
oBaking is 1 hour in the tube furnace of C, uses oxyhydrogen flame sealing-in ampoule then; The quartz ampoule that the glass compound is housed that sealing-in is good is put into and is waved stove, slowly is warming up to 800
oC is incubated to take out after 10 hours and cools off in air, then 132
oC annealing 2 hours; The ampoule that fills glass after the annealing is opened in glove box, taken out glass, in the open type of packing into the still tube, then glass is carried out open type and dynamically distill; The silica tube that distillation back mixture is housed put into wave stove, slowly be warming up to 800
oC is incubated to take out after 8 hours and cools off in air, then 132
oC annealing 5 hours is at last with 0.2
oThe speed of C/min drops to room temperature.Become thickness to be respectively 2mm the glass cutting that finally obtains, the sheet glass of 5mm and 10mm and twin polishing adopt the high resolving power infrared camera sight glass inside that is operated in 7.5-13 μ m whether to have micron-sized heterogeneous inclusion; Detect the infrared transmission spectra of above-mentioned three kinds of thickness glass sheets, adopt the cut-back method to calculate the loss of glass; Adopt X-ray energy spectrometer to detect the variation of glass purification front and back component; Adopting service band is the specific refractory power of the infrared ellipsometer tested glass distillation front and back of 1.7-30 μ m; Detected result shows: glass is observed the heterogeneous inclusion of no obvious micron order under the high resolving power infrared camera; The final highly pure glass that obtains is 0.2dB/m in the lowest loss of infrared permeation wave band, and the corresponding loss of residual impurity absorption peak (Se-H, 4.53 μ m) is 6.0dB/m; Form before and after the glass distillation and be respectively Te
20.2As
30.1Se
49.7And Te
20.1As
30.0Se
49.9Specific refractory power at 5.3 mum wavelengths before and after the glass distillation is respectively 2.927 ± 0.002,2.926 ± 0.001.
Claims (4)
1. the preparation method of a high-purity low-loss chalcogenide glass is characterized in that: the preparation method introduces the super dried gallium chloride (GaCl of 200-2000ppm mol ratio in the chalcogenide glass system
3) as the purifying agent of dehydrogenation and carbon impurity, introduce aluminium (Al), magnesium (Mg) or the zirconium (Zr) of 100-500ppm mol ratio as oxygen scavenger, purify by the method for dynamic distillation, obtain uniform high-purity chalcogenide glass; Concrete steps are as follows:
(1) preparation of glass compound
Form proportioning formulate glass compound in the district with the simple substance element of purity 〉=99.999% by corresponding glass, add glassivation agent and the 100-500ppm oxygen scavenger of 200-2000ppm; Blending process carries out in the inert environments of drying, and the compound hydroxy radical content of packing into is lower than in the clean quartz ampoule of 1ppm;
(2) vacuumize sealing-in
To vacuumize vacuum tightness in ampoule≤10 by the quartz ampoule that step (1) gained fills compound
– 3During Pa, ampoule is placed on 100-150
oBaking is 1-4 hour in the tube furnace of C, uses oxyhydrogen flame sealing-in ampoule then;
(3) glass smelting
To be put into by the good quartz ampoule that the glass compound is housed of step (2) gained sealing-in and wave stove, slowly be warming up to 800 ~ 950
oC is incubated and takes out cooling after 10 ~ 20 hours, anneals near the glass transformation temperature of correspondence then 2-5 hour;
(4) distillation of glass
The distillation of glass is carried out in the open type still tube, and the open type still tube is connected to form by a kapillary by material feeding region A and discharge zone B; The ampoule that step (3) gained is filled glass is opened in the inert environments of drying, takes out glass, the material feeding region A of the open type of packing into still tube; With soft rubber ball discharge port is blocked, vacuumized from feeding mouth, when vacuum tightness≤10
– 3During Pa from feeding mouth rear end sealing-in still tube; Still tube is put into a two warm area tube furnace, take off the discharge port soft rubber ball, and from then on end vacuumizes, when vacuum tightness≤10
– 3During Pa, slowly material feeding region A is warming up to 700-800
oC also is incubated 1 hour, simultaneously discharge zone B slowly is warming up to 200-550
oC; Glass can slowly be distilled to discharging B from material feeding region A, and the oxide impurity of low-steam pressure can be stayed material feeding region A, high-volatile HCl, CCl
4Can be taken away from discharge port Deng impurity, the glass that vapour pressure is moderate is stayed discharge zone B; Then respectively from discharge zone rear end and discharge zone front end sealing-in silica tube, the mixture after obtaining distilling;
(5) remelting of glass
The silica tube that step (4) gained is filled distillation back mixture is put into and is waved stove, slowly is warming up to 800 ~ 950
oC is incubated and takes out cooling after 8-12 hour, anneals near the glass transformation temperature of correspondence then 2-5 hour, slowly drops to room temperature at last, namely obtains high-purity low-loss chalcogenide glass.
2. require the preparation method of 1 described a kind of high-purity low-loss chalcogenide glass according to power, it is characterized in that: described chalcogenide glass is to be the chalcogenide glass of component with the two or more elements in germanium, arsenic, antimony, sulphur, selenium and the tellurium; Described glassivation agent is super dried gallium chloride; Described oxygen scavenger is aluminium, magnesium or zirconium metal.
3. require the preparation method of 1 described a kind of high-purity low-loss chalcogenide glass according to power, it is characterized in that: raw materials usedly be the high pure element of purity 〉=99.999%.
4. require the preparation method of 1 described a kind of high-purity low-loss chalcogenide glass according to power, it is characterized in that: the glass distillating method that adopts is the dynamic distillating method of open type.
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