CN204529642U - Chalcogenide glass preparation facilities - Google Patents
Chalcogenide glass preparation facilities Download PDFInfo
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- CN204529642U CN204529642U CN201420869703.3U CN201420869703U CN204529642U CN 204529642 U CN204529642 U CN 204529642U CN 201420869703 U CN201420869703 U CN 201420869703U CN 204529642 U CN204529642 U CN 204529642U
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Abstract
The utility model is about a kind of chalcogenide glass preparation facilities, expect that forming furnace is communicated with by vacuum melting stove and leakage to form, vacuum melting stove comprises smelting furnace body of heater, quartz crucible, heating unit, jacking system, whipping appts, vacuum system, inlet mouth and crucible gland; Smelting furnace body of heater is made up of upper and lower bell and middle part furnace chamber; Quartz crucible is positioned at above lower bell, and described quartz crucible side lower is provided with a leakage material mouth, stretches into and Lou expects in shaping body of heater; Heating unit, is assemblied on the furnace chamber wall of middle part, is looped around crucible surrounding; Jacking system is used for carrying out descending operation to quartz crucible; Whipping appts, is assemblied in bell, for carrying out high-temperature stirring to glass metal, adopts high purity quartz to make; Vacuum system, is made up of vacuum pipe and multistage vacuum pump, takes out vacuum processed by vacuum pump to closed furnace body; Inlet mouth, is positioned at bottom, furnace wall, middle part.Device of the present utility model can prepare that optical homogeneity is good, spectral transmission excellent performance, large-sized chalcogenide glass.
Description
Technical field
The utility model relates to a kind of glass preparation device, particularly relates to a kind of suitable large size, high evenly chalcogenide glass preparation facilities.
Background technology
Glasses for infrared use are the special glass materials with infrared transmission performance, compared to the crystal such as monocrystalline, polycrystalline class infra-red material, have optical homogeneity good, be easy to the features such as preparation, particularly can carry out shaping and the processing of large size and special-shaped infrared device, become one of emphasis of infra-red material research application.
Chalcogenide glass refers to based on the periodic table of elements VI A race element S, Se, Te introduce the glass that other elements a certain amount of are formed.For oxide glass, chalcogenide glass has larger quality and more weak key is strong, is a kind of excellent infrared optical material, spectral transmission scope (0.9 ~ 15 μm).Chalcogenide glass is as a kind of infrared optical material, wide through spectral range at infrared band with it, Photothermal characterisation is stablized, chemical stability is excellent, performance continuously adjustabe, the low easy processing of preparation cost and there is the advantages such as complementary in some performances with the infrared crystal material such as monocrystalline germanium, in IR optical component design, heat differs from the low chalcogenide glass of coefficient and Gao Re differs from coefficient crystalline material Combination application and infrared optical system, can the range of choice of extreme enrichment infrared optical material, increase the handiness of system design, simplied system structure, what is more important significantly can improve the image quality of system (-55 DEG C ~ 130 DEG C) under various circumstances, promote the temperature self-adaptation performance of the optical systems such as infrared thermal imaging, meet system without thermalized design requirement, therefore, chalcogenide glass is regarded as temperature self-adaptation infrared optical system core lens material of new generation, can be widely used in that military (night vision rifle is taken aim at, infrared guided missile pickaback, opportunity of combat night vision is cruised) and civilian (vehicle night vision, safety monitoring etc.) in infrared system, its market outlook are huge.
Chalcogenide glass is in preparation process, very easily be subject to the pollution of ambient impurities and moisture, the glass prepared is made to occur strong Impurity Absorption peak at places such as infrared 2.9 μm, 4.1 μm, 4.5 μm, 6.3 μm and 12.8 μm, thus affect the infrared spectra performance of glass, cause overall infrared transmittivity to decline.The Impurity Absorption peak how eliminated in glass preparation process becomes gordian technique and difficult point prepared by high quality glasses for infrared use; The defects such as the striped that chalcogenide glass produces in preparation process, furuncle knurl have a strong impact on the internal soundness of glass.In addition, the preparation of tradition chalcogenide glass has very strong technique singularity, it generally needs to carry out high temperature in the airtight quartz ampoule bottle of the cylindricity of anaerobic high vacuum atmosphere and waves and found, chalcogenide glass prepared by this method has the shortcomings such as inboard stripes defect is more, the little and batch instability of preparation specimen size, the size of the chalcogenide glass prepared in prior art is general all at 100 × below 100mm, then very difficult more than the chalcogenide glass of 100 × 100mm for preparation.
Utility model content
Main purpose of the present utility model is, provides a kind of chalcogenide glass preparation facilities, and technical problem to be solved to prepare large-sized chalcogenide glass goods.
The purpose of this utility model and solve its technical problem and adopt following technical scheme to realize.According to the preparation facilities of a kind of chalcogenide glass that the utility model proposes, be characterised in that and form by being communicated with leakage material forming furnace two part, wherein vacuum melting stove comprises: smelting furnace body of heater, quartz crucible, heating unit, jacking system, whipping appts, vacuum system, inlet mouth and crucible gland; Wherein: smelting furnace body of heater, be made up of upper and lower bell and middle part furnace chamber, upper and lower bell all can be opened, and upper cover is used for reinforced, and lower cover is used for safeguarding at ordinary times; Quartz crucible, for holding glass metal, is positioned at above lower bell; Crucible gland, is positioned at above crucible, for preventing glass metal volatility of raw material and splashing, is made up of high purity quartz; Heating unit, is assemblied on the furnace chamber wall of middle part, is looped around crucible surrounding; Jacking system, for carrying out descending operation to quartz crucible; Whipping appts, is assemblied in bell, for carrying out high-temperature stirring to glass metal, adopts high purity quartz to make; Vacuum system, is made up of vacuum pipe and multistage vacuum pump, and vacuum pipe is communicated in furnace wall, middle part, is vacuumized closed furnace body by vacuum pump; Inlet mouth, is positioned at bottom, furnace wall, middle part, for stove interacvity air-filling.
Further, in aforesaid preparation facilities, described leakage material forming furnace comprises: leak material shaping body of heater, be communicated with described smelting furnace body of heater, described quartz crucible side lower is provided with a leakage material mouth, and stretches in described leakage material shaping body of heater; Found baffle plate, be arranged on described leakage material mouth, for opening or closed leakage material mouth; Heater coil, is arranged on around described leakage material mouth, for heating leakage material mouth; Leak material shaping mobile system, be arranged on and Lou expect in shaping body of heater; With leakage material shaping dies, be arranged on described leakage material shaping mobile system.
By technique scheme, the utility model chalcogenide glass preparation facilities at least has following advantages:
A kind of chalcogenide glass preparation facilities disclosed in the utility model, it can be prepared by " vacuum and low temperature process+vacuum high-temperature is founded+leaked material and is shaped " three-step approach, and optical homogeneity is good, spectral transmission excellent performance, large-sized chalcogenide glass goods.Scheme of the present utility model improves the through performance of infrared chalcogenide glass at 0.9 ~ 13 μm of infrared band greatly, greatly improves the practical level of chalcogenide glass.
Above-mentioned explanation is only the general introduction of technical solutions of the utility model, in order to better understand technique means of the present utility model, and can be implemented according to the content of specification sheets, coordinates accompanying drawing to be described in detail as follows below with preferred embodiment of the present utility model.
Accompanying drawing explanation
Fig. 1 is that material forming furnace structural representation is leaked in the utility model vacuum melting;
Fig. 2 is the infrared spectra curve that the utility model method prepares chalcogenide glass;
Fig. 3 is the visible region curve of spectrum that the utility model method prepares chalcogenide glass;
The comparison of the chalcogenide glass that Fig. 4 is prepared for the utility model method and chalcogenide glass infrared perspective image prepared by conventional melt quenching technology, a) the infrared perspective image of conventional melt quenching technology chalcogenide glass; B) the chalcogenide glass infrared perspective image prepared of the utility model method;
Fig. 5 embodiment 1 obtains the infrared penetrating image forming figure of chalcogenide glass;
The chalcogenide glass infrared penetrating image forming figure that Fig. 6 embodiment 2 is obtained.
Embodiment
For further setting forth the utility model for the technique means reaching predetermined utility model object and take and effect, below in conjunction with accompanying drawing and preferred embodiment, to according to its embodiment of chalcogenide glass preparation facilities, structure, feature and the effect thereof that the utility model proposes, be described in detail as follows.
Referring to shown in Fig. 1, is the preparation facilities of a kind of chalcogenide glass that the utility model embodiment provides, for large size, the preparation of high evenly chalcogenide glass.This preparation facilities comprises chalcogenide glass vacuum melting stove and leaks material forming furnace, and described chalcogenide glass vacuum melting stove and leakage material forming furnace are interconnected, and jointly form enclosed space.Described chalcogenide glass vacuum melting stove, for melting chalcogenide glass, it comprises smelting furnace body of heater 11, quartz crucible 12, heating unit 14, jacking system 15, whipping appts 16, vacuum system 17, inlet mouth 18 and crucible gland 19.Wherein: smelting furnace body of heater 11 is made up of upper bell, lower bell and middle part furnace chamber, material is heat-resistance stainless steel, and upper and lower bell all can be opened, and upper bell is used for reinforced, and lower bell is used for safeguarding at ordinary times.Described jacking system 15 is for carrying out descending operation to quartz crucible 12, and it is arranged on lower bell.Described quartz crucible 12, for holding high temp glass liquid 13, is positioned at above lower bell, is carried by jacking system, and can with lower furnace cover lifting.Described crucible gland 19 is positioned at above crucible, for preventing volatility of raw material, glass metal from splashing, is made up of high purity quartz; Described heating unit 14 is heater coil, is assemblied on the furnace chamber wall of middle part, is looped around crucible surrounding, heats material; Preferably, described heating unit 14 can realize top temperature 1200 DEG C, the temperature difference can control ± 2 DEG C within.Described whipping appts 16 is assemblied in bell, and for carrying out high-temperature stirring to glass metal, for avoiding introducing impurity in glass, the same high purity quartz that adopts is made; Described vacuum system 17 is made up of vacuum pipe and multistage vacuum pump, and vacuum pipe is communicated in furnace wall, middle part, is vacuumized, can realize high vacuum 5 × 10 by vacuum pump to closed furnace body
-5pa.Described inlet mouth 18 is positioned at bottom, furnace wall, middle part, for having melted rear unlatching air valve to stove interacvity air-filling, recovers furnace chamber pressure to normal pressure.
Described leakage material forming furnace comprises leakage material shaping body of heater 20, founds baffle plate 21, heater coil 22, leaks material mouth 23, leaks and expect shaping dies 24 and leak material shaping mobile system 25.Described leakage material shaping body of heater 20 is communicated with described smelting furnace body of heater.Described quartz crucible 12 lower sidewall is provided with a leakage material mouth 23, and this leakage material mouth 23 stretches in described leakage material shaping body of heater; Described founds baffle plate 21, is arranged on described leakage material mouth, for opening or closed leakage material mouth; Described heater coil 22, is arranged on around described leakage material mouth, for heating leakage material mouth; Described leakage material shaping mobile system 25, is arranged on and Lou expects bottom in shaping body of heater; Leak material shaping dies 24, be arranged on described leakage material shaping mobile system.Driven by described leakage material shaping mobile system 25 and Lou expect that shaping dies 24 moves, thus the glass metal that leakage material mouth leaks down is paved on leakage material shaping dies 24, form glassy product.Preferably, described leakage material shaping dies 24 has heating unit and temperature-control device, thus accurately can control the temperature of glass metal in mould and mould.The size of leaking material shaping dies 24 is greater than 250 × 250mm, thus can preparation size be the glass finished-product of (100 ~ 250) × (100 ~ 250) mm.
Chalcogenide glass preparation facilities described in the present embodiment, can to realize under 400 ~ 1200 DEG C of hot conditionss at vacuum environment purifying and found, meeting the needs that large size chalcogenide glass goods found operation.Described chalcogenide glass preparation facilities has the advantages such as device structure is simple, easy care, mechanical stirring under vacuum melt environment, not only be conducive to the homogenizing of glass, also the eliminating of the impurity such as hydroxyl and bubble in glass is conducive to, the optical quality of further raising glass and spectral transmission performance, be applicable to the preparation of the infrared chalcogenide glass of high quality.Leakage material forming furnace in the utility model embodiment by the control realization of heater coil and baffle plate to leaking material speed, leaking the control of material process, leak material in vacuum environment under can realizing 200 ~ 600 DEG C of temperature condition, meet the needs that large size chalcogenide glass goods leak material forming operation.Burst the generation of situation additionally by effectively can reduce chalcogenide glass when leakage is expected to the control of die temperature, and realize the black annealing to chalcogenide glass.
Embodiment of the present utility model also proposes a kind of suitable large size, high evenly chalcogenide glass preparation method, and preferably adopt above-mentioned chalcogenide glass preparation facilities, the method comprises following three steps: vacuum and low temperature purifying, under vacuum, at the first temperature T
1under purifying is carried out to frit, remove impurity; Vacuum high-temperature is founded, under vacuum, at the second temperature T
2under make frit fusing obtain the glass metal of molten state; Leak material to be shaped, the glass metal of molten state is spilt, and shaping, obtain glass finished-product; Described vacuum condition is that pressure is less than 1.0 × 10
-2pa.Preferably, the purity of described frit is 5N level.The selection of described frit should meet makes final chalcogenide glass be made up of following material: one or both in Ge element and As element, and its molar content is 5 ~ 35%; Sb element, its molar content is 5 ~ 40%; Al element or Mg element, its molar content is 50 ~ 200ppm; Be one or both in Se element and Te element with surplus.
Further, described vacuum and low temperature purifying comprises: be placed in by frit in smelting furnace, vacuumize smelting furnace, makes smelting furnace internal pressure be less than 5 × 10
-3pa; Heating, makes fusing in-furnace temperature at 200 ~ 400 DEG C, keeps more than 3 hours.
Described vacuum high-temperature is founded and is comprised: be warming up to 800 ~ 1000 DEG C, and controlled melting furnace pressure is less than 1 × 10
-2pa, carries out batch type to frit in the process.After described high temperature melting, leave standstill 0.5 ~ 1h; And then carrying out the shaping of leakage material, described glass finished-product is of a size of (100 ~ 250) × (100 ~ 250) mm.Described formula of having a rest mechanical stirring technique is: stir 10 ~ 20min, and rear standing 30 ~ 50min, so repeats 2 ~ 5 times.
As shown in Figures 2 to 4, described chalcogenide glass is that the transmitance at 2.9 μm, 4.1 μm, 4.5 μm, 6.3 μm places is more than 63% at wavelength; Wavelength 12.8 μm place transmitance is more than 50%, and the display of infrared perspective image does not have obvious strip flaw, very evenly.
According to above-mentioned chalcogenide glass preparation method, prepare following instance.
Example 1
Take chalcogenide glass raw material with the accurate proportioning of 28mol%, 60mol% and 12mol% respectively according to germanium, selenium, antimony simple substance and make compound 1, oxygen scavenger aluminium 200ppm is introduced to above-mentioned compound 1, compound 1 is loaded in the quartz crucible 12 of vacuum melting stove, vacuumized, to 5 × 10 by vacuum melting stove 17 position
-3about Pa, coil 14 starts heating, is warming up to T in 0.5h
1=350 DEG C of purifying 2h.After purifying terminates, be rapidly heated: be warming up to T with 10 DEG C/min speed
2=950 DEG C, and at this temperature 4h.Insulation starts to introduce quartzy agitator in glass metal, and carry out glass metal homogenization operation, stirring velocity is 10rpm/min, and stirring technique system is: stir 10min, rear standing 20min, repeat 3 times.After insulation terminates, stop stirring, mention agitator, be down to drop temperature 580 DEG C with 10 DEG C/min rate of temperature fall, insulation 2h.When insulation terminates front 45min, start to add heat leak flitch and coil.At the end of insulation, after the glass leaked in material mouth melts completely, promote baffle plate, carry out the operation of leakage material, preparation 150 × 150mm specification glass sheet material, the translational speed of leaking flitch is 10cm/min.Leak material to terminate, closing baffle plate, leakage material mouth is cooled.
The glass that said process obtains, after fine annealing, is processed into 30 × 20 × 2mm glass print, and spectrum property detection is carried out in surface after polishing, as shown in Figures 2 and 3, and Ge
28se
60sb
12glass print detected result shows, through performance: 900 ~ 1000nm, transmitance>=63%; Wavelength is 2.9 μm of place's transmitances is 63%; Wavelength is 4.1 μm of place's transmitances is 63%; Wavelength is 4.5 μm of place's transmitances is 63%; Wavelength is 6.3 μm of place's transmitances is 63%; 12.8 μm of place's transmitances are 58%.Adopt infrared penetrating image forming systematic observation internal soundness, see Fig. 5.
Found rear obtained Ge
28se
60sb
12frit, other physicochemical properties are in table 2.
Table 2, vacuum melt Ge
28se
60sb
12chalcogenide glass main performance index
Example 2:
Accompanying drawing 1 shown device purifying is used to found Ge
20se
65sb
15frit, take 5000g raw material and oxygen scavenger aluminium 100ppm with the accurate proportioning of 20mol%, 65mol% and 15mol% respectively according to germanium, selenium, antimony simple substance and be used as compound 1, compound 1 is loaded in the quartz crucible 12 of vacuum melting stove, undertaken being evacuated to 6 × 10 by vacuum melting stove 17 position
-4about Pa, heats coil 4, is warming up to T in half an hour
1=300 DEG C of purifying 2h.Purifying is rapidly heated after terminating: be warming up to T with 8 DEG C/min speed
2=930 DEG C, and 5h is incubated under this temperature condition.Insulating process carries out homogenization operation by quartzy mechanical stirring device to glass metal, and stirring velocity is 10rpm/min, and stirring technique system is: stir 20min, rear standing 20min, repeat 2 times.After insulation terminates, stop stirring, mention agitator, be down to drop temperature 580 DEG C with 10 DEG C/min rate of temperature fall, insulation 2h.When insulation terminates front 30min, start to add heat leak flitch and coil.At the end of insulation, after the glass leaked in material mouth melts completely, promote baffle plate, carry out the operation of leakage material, preparation 250 × 200mm specification glass sheet material, the translational speed of leaking flitch is 10cm/min.Leak material to terminate, closing baffle plate, leakage material mouth is cooled.
Carry out Performance Detection with example 1 same procedure sample preparation.
Example 2 glass print detected result shows, through performance: 900 ~ 1100nm, transmitance >=63%; Wavelength is 2.9 μm of place's transmitances is 64%; Wavelength is 4.1 μm of place's transmitances is 63%; Wavelength is 4.5 μm of place's transmitances is 64%; Wavelength is 6.3 μm of place's transmitances is 64%; 12.8 μm of place's transmitances are 58%.Adopt infrared penetrating image forming systematic observation internal soundness, see Fig. 6.
Found rear obtained Ge
20se
65sb
15frit, other physicochemical properties are in table 3.
Table 3, vacuum melt Ge
20se
65sb
15chalcogenide glass main performance index
As shown in Figure 4, the comparison of chalcogenide glass prepared by the utility model method and chalcogenide glass infrared perspective image prepared by conventional melt quenching technology, a) the infrared perspective image of conventional melt quenching technology chalcogenide glass, has obvious strip flaw; B) the chalcogenide glass infrared perspective image prepared of the utility model method, does not have obvious strip flaw.
Above embodiment shows, the preparation method of a kind of large size that the utility model proposes, high evenly chalcogenide glass and preparation facilities solve the impurity expeling of chalcogenide glass and a difficult problem for high temperature homogenizing, coordinate suitable leakage material to be shaped, the preparation of≤large size such as Φ 200mm bore lens, 250 × 250mm optical window, high quality chalcogenide glass device blank can be carried out.
The above, it is only preferred embodiment of the present utility model, not any pro forma restriction is done to the utility model, although the utility model discloses as above with preferred embodiment, but and be not used to limit the utility model, any those skilled in the art, do not departing within the scope of technical solutions of the utility model, make a little change when the technology contents of above-mentioned announcement can be utilized or be modified to the Equivalent embodiments of equivalent variations, in every case be the content not departing from technical solutions of the utility model, according to any simple modification that technical spirit of the present utility model is done above embodiment, equivalent variations and modification, all still belong in the scope of technical solutions of the utility model.
Claims (2)
1. the preparation facilities of a chalcogenide glass, it is characterized in that, expect that forming furnace two part is communicated with by vacuum melting stove and leakage to form, described vacuum melting stove comprises: smelting furnace body of heater, quartz crucible, heating unit, jacking system, whipping appts, vacuum system, inlet mouth and crucible gland; Wherein:
Smelting furnace body of heater, be made up of upper and lower bell and middle part furnace chamber, upper and lower bell all can be opened, and upper cover is used for reinforced, and lower cover is used for safeguarding at ordinary times; Quartz crucible, for holding high temp glass liquid, is positioned at above lower bell, and described quartz crucible side lower is provided with a leakage material mouth, stretches in described leakage material shaping body of heater; Crucible gland, is positioned at above crucible, for preventing volatility of raw material, glass metal from splashing, is made up of high purity quartz; Heating unit, is assemblied on the furnace chamber wall of middle part, is looped around crucible surrounding; Jacking system, for carrying out descending operation to quartz crucible; Whipping appts, is assemblied in bell, for carrying out high-temperature stirring to glass metal, adopts high purity quartz to make; Vacuum system, is made up of vacuum pipe and multistage vacuum pump, and vacuum pipe is communicated in furnace wall, middle part, takes out vacuum processed by vacuum pump to closed furnace body; Inlet mouth, is positioned at bottom, furnace wall, middle part, for stove interacvity air-filling.
2. the preparation facilities of chalcogenide glass according to claim 1, it is characterized in that, described leakage material forming furnace is communicated with described smelting furnace body of heater, and this leakage material forming furnace comprises: leak material shaping body of heater, found baffle plate, heater coil, leakage material shaping mobile system, leak material shaping dies; Wherein:
Leak material shaping body of heater, be made up of upper and lower bell and middle part furnace chamber, upper and lower bell all can be opened; Found baffle plate, be arranged on described leakage material mouth, for opening or closed leakage material mouth; Heater coil, is arranged on around described leakage material mouth, for heating leakage material mouth; Leak material shaping mobile system, be arranged on and Lou expect in shaping body of heater; With leakage material shaping dies, be arranged on described leakage material shaping mobile system.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104556633A (en) * | 2014-12-31 | 2015-04-29 | 中国建筑材料科学研究总院 | Preparation method and preparation device for chalcogenide glass |
| CN105450164A (en) * | 2015-11-28 | 2016-03-30 | 李白 | Ultra-large type solar energy power generation device |
| CN108726850A (en) * | 2018-06-25 | 2018-11-02 | 中国建筑材料科学研究总院有限公司 | Pressure controls glass melting device and method |
| CN115321810A (en) * | 2022-08-19 | 2022-11-11 | 北京科技大学 | Preparation method of glass optical fiber |
-
2014
- 2014-12-31 CN CN201420869703.3U patent/CN204529642U/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104556633A (en) * | 2014-12-31 | 2015-04-29 | 中国建筑材料科学研究总院 | Preparation method and preparation device for chalcogenide glass |
| CN105450164A (en) * | 2015-11-28 | 2016-03-30 | 李白 | Ultra-large type solar energy power generation device |
| CN108726850A (en) * | 2018-06-25 | 2018-11-02 | 中国建筑材料科学研究总院有限公司 | Pressure controls glass melting device and method |
| CN108726850B (en) * | 2018-06-25 | 2021-03-26 | 中国建筑材料科学研究总院有限公司 | Pressure-controlled glass melting device and method |
| CN115321810A (en) * | 2022-08-19 | 2022-11-11 | 北京科技大学 | Preparation method of glass optical fiber |
| CN115321810B (en) * | 2022-08-19 | 2023-09-19 | 北京科技大学 | Preparation method of glass optical fiber |
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