CN107056016A - Chalcogenide glass and preparation method thereof and device - Google Patents
Chalcogenide glass and preparation method thereof and device Download PDFInfo
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- CN107056016A CN107056016A CN201710375991.5A CN201710375991A CN107056016A CN 107056016 A CN107056016 A CN 107056016A CN 201710375991 A CN201710375991 A CN 201710375991A CN 107056016 A CN107056016 A CN 107056016A
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- 239000005387 chalcogenide glass Substances 0.000 title claims abstract description 88
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 230000006698 induction Effects 0.000 claims abstract description 75
- 238000002844 melting Methods 0.000 claims abstract description 59
- 230000008018 melting Effects 0.000 claims abstract description 59
- 238000010438 heat treatment Methods 0.000 claims abstract description 53
- 238000001816 cooling Methods 0.000 claims abstract description 34
- 239000011521 glass Substances 0.000 claims abstract description 26
- 238000000265 homogenisation Methods 0.000 claims description 44
- 238000000034 method Methods 0.000 claims description 35
- 239000000463 material Substances 0.000 claims description 30
- 239000002994 raw material Substances 0.000 claims description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 20
- 238000012546 transfer Methods 0.000 claims description 17
- 230000005540 biological transmission Effects 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 13
- 238000009413 insulation Methods 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 238000000746 purification Methods 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 229940123973 Oxygen scavenger Drugs 0.000 claims description 5
- 239000004615 ingredient Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000003723 Smelting Methods 0.000 abstract description 12
- 239000000203 mixture Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000009740 moulding (composite fabrication) Methods 0.000 description 8
- 239000003708 ampul Substances 0.000 description 7
- 238000003384 imaging method Methods 0.000 description 6
- 238000000137 annealing Methods 0.000 description 4
- 238000007664 blowing Methods 0.000 description 4
- 150000004770 chalcogenides Chemical class 0.000 description 4
- 229910052732 germanium Inorganic materials 0.000 description 4
- 238000010309 melting process Methods 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 239000006060 molten glass Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000010923 batch production Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000001931 thermography Methods 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000003044 adaptive effect Effects 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
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000003331 infrared imaging Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000000075 oxide glass Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/02—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture in electric furnaces, e.g. by dielectric heating
- C03B5/021—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture in electric furnaces, e.g. by dielectric heating by induction heating
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
- C03B5/18—Stirring devices; Homogenisation
- C03B5/183—Stirring devices; Homogenisation using thermal means, e.g. for creating convection currents
- C03B5/185—Electric means
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
- Glass Compositions (AREA)
Abstract
本发明提供了一种硫系玻璃及其制备方法和制备装置，其中，装置包括，熔化模块、升降模块、均化模块、冷却模块、传送模块和坩埚，其中，所述的熔化模块包括炉盖、炉体、中频感应线圈和感应发热体，所述的炉盖和炉体构成熔化腔体，所述的熔化腔体底部开口，所述的中频感应线圈位于所述的熔化腔体内所述的升降模块用于带动所述的坩埚做第一运动；所述的均化模块包括保温炉和温度控制系统。本发明有效解决了硫系玻璃现有技术熔炼效率低、组成性能一致性控制难度大等问题，可很好地实现高质量硫系玻璃的高效熔炼和批量制备，进一步提高红外玻璃的实用化水平。
The invention provides a chalcogenide glass and its preparation method and preparation device, wherein the device includes a melting module, a lifting module, a homogenizing module, a cooling module, a conveying module and a crucible, wherein the melting module includes a furnace cover , a furnace body, an intermediate frequency induction coil and an induction heating body, the furnace cover and the furnace body constitute a melting cavity, the bottom of the melting cavity is open, and the intermediate frequency induction coil is located in the melting cavity The lifting module is used to drive the crucible to perform the first movement; the homogenizing module includes a holding furnace and a temperature control system. The present invention effectively solves the problems of low smelting efficiency of chalcogenide glass in the prior art and difficulty in controlling the consistency of composition performance, etc., can well realize high-efficiency smelting and batch preparation of high-quality chalcogenide glass, and further improves the practical level of infrared glass .
Description
技术领域technical field
本发明涉及红外玻璃制备技术领域，特别是涉及一种高质量硫系玻璃的高效熔炼、批量生产装置、制备方法以及制备得到的硫系玻璃。The invention relates to the technical field of infrared glass preparation, in particular to a high-efficiency smelting of high-quality chalcogenide glass, a batch production device, a preparation method and the prepared chalcogenide glass.
背景技术Background technique
硫系玻璃是一种性能优良的红外透过材料，其组成以第VIA族元素(S、Se等)为主，通过引入Ge、Sb、As等元素而形成。硫系玻璃具有类似于单晶锗的中远红外透过性能，红外透过范围覆盖1～14μm波段三个红外大气窗口；同时具有较好的光-热稳定特性，折射率温度系数低，(单晶锗的10％～30％)且可调，有利于提高红外热成像光学系统的温度自适应能力，满足无热化红外光学设计要求。硫系红外玻璃可有效降低对锗等资源的消耗，实现红外透镜的低成本制造，另外，硫系玻璃还可采用精密模压技术成形，进一步降低加工成本。基于以上特点，硫系玻璃已被视为新一代无热化红外成像光学系统核心透镜材料，在红外成像制导、夜视枪瞄、汽车夜视辅助驾驶、安防监控等国防、民用红外技术领域应用前景广阔。Chalcogenide glass is a kind of infrared transparent material with excellent performance. Its composition is mainly composed of group VIA elements (S, Se, etc.), and it is formed by introducing elements such as Ge, Sb, and As. Chalcogenide glass has mid-to-far infrared transmission performance similar to that of single crystal germanium, and the infrared transmission range covers three infrared atmospheric windows in the 1-14 μm band; at the same time, it has good light-thermal stability characteristics, low temperature coefficient of refraction index, (single 10% to 30% of crystal germanium) and adjustable, which is conducive to improving the temperature adaptive ability of the infrared thermal imaging optical system and meeting the design requirements of athermal infrared optics. Chalcogenide infrared glass can effectively reduce the consumption of resources such as germanium and realize low-cost manufacturing of infrared lenses. In addition, chalcogenide glass can be formed by precision molding technology to further reduce processing costs. Based on the above characteristics, chalcogenide glass has been regarded as the core lens material of a new generation of athermal infrared imaging optical system. Broad prospects.
硫系玻璃是一种非氧化物玻璃材料，其熔炼工艺具有很强的特殊性，必须在真空或气氛保护环境下进行，以防止氧化及氢、碳环境杂质的污染对红外透过性能的影响。目前采用的方法主要是安瓿瓶摇摆法。Chalcogenide glass is a kind of non-oxide glass material. Its smelting process has strong specificity and must be carried out in a vacuum or atmosphere protection environment to prevent the influence of oxidation, hydrogen and carbon environmental impurities on the infrared transmission performance. . The method currently used is mainly the ampoule rocking method.
安瓿瓶摇摆法可以追溯至上世纪60年代，即是将硫系玻璃原料真空密封在石英安瓿瓶中，然后将石英安瓿瓶在摇摆炉内升温熔化，期间通过炉体的摇摆来对安瓿瓶内的玻璃液进行均化，熔炼完成后对安瓿瓶进行淬冷降温，得到硫系玻璃毛坯。该方法过程简单，玻璃光谱性能好，但是受到石英安瓿瓶及摇摆熔化方式的限制，存在生产周期长、光学均匀性差、产能小、制品尺寸小等缺点。随着硫系玻璃需求量及对性能要求的不断提高，该方法逐渐无法满足应用需求。The ampoule swing method can be traced back to the 1960s, that is, the chalcogenide glass raw material is vacuum-sealed in a quartz ampoule, and then the quartz ampoule is heated and melted in a swing furnace. The molten glass is homogenized, and after the smelting is completed, the ampoule is quenched and cooled to obtain a chalcogenide glass blank. This method has simple process and good spectral performance of glass, but it is limited by quartz ampoule and swing melting method, and has disadvantages such as long production cycle, poor optical uniformity, small production capacity, and small product size. As the demand for chalcogenide glass and the performance requirements continue to increase, this method is gradually unable to meet the application requirements.
针对上述情况，国内外相继开发了其他硫系玻璃的熔炼方法，以期改善生产效率、提高产品性能。美国AMI(Amorphous Materials)公司、比利时Umicore公司等发明了硫系玻璃气氛保护熔制方法，通过在反应熔体上方设定适宜的正压等措施控制Se等原料的挥发，利用机械搅拌进行玻璃的熔化澄清，最后通过漏料得到硫系玻璃。现有技术中，利用安瓿瓶法获得硫系玻璃熟料，然后在气氛保护熔制炉内对硫系玻璃熟料进行二次均化，最后由坩埚底部漏料成形硫系玻璃产品。In response to the above situation, other chalcogenide glass melting methods have been developed at home and abroad in order to improve production efficiency and product performance. AMI (Amorphous Materials) Company of the United States, Umicore Company of Belgium, etc. have invented the atmosphere protection melting method of chalcogenide glass, by setting a suitable positive pressure above the reaction melt to control the volatilization of raw materials such as Se, and using mechanical stirring to carry out glass melting. It is melted and clarified, and finally chalcogenide glass is obtained through leakage. In the prior art, the chalcogenide glass clinker is obtained by using the ampoule method, and then the chalcogenide glass clinker is homogenized for the second time in the atmosphere protection melting furnace, and finally the chalcogenide glass product is formed by leaking material from the bottom of the crucible.
以上方法打破了摇摆法对玻璃制品尺寸、形状、性能和产量等方面的限制，显著改善了硫系玻璃的生产能力和产品规格尺寸。但上述制备方法装置结构复杂，对反应温度、压力等监测要求较高，工艺难度大。并且一旦原料挥发控制不好或杂质引入，会引起硫系玻璃制品组成和性能的波动，熔炼批次稳定性差，影响热成像等红外光电系统的性能和应用。The above method breaks the limitations of the rocking method on the size, shape, performance and output of glass products, and significantly improves the production capacity and product specifications of chalcogenide glass. However, the device structure of the above-mentioned preparation method is complex, the monitoring requirements for reaction temperature and pressure are relatively high, and the process is difficult. And once the volatilization of raw materials is not well controlled or impurities are introduced, it will cause fluctuations in the composition and performance of chalcogenide glass products, poor stability of smelting batches, and affect the performance and application of infrared photoelectric systems such as thermal imaging.
发明内容Contents of the invention
本发明的主要目的在于，提供一种硫系红外玻璃的感应熔炼设备、熔炼方法以及其制备得到的硫系红外玻璃，通过特殊设计的炉体结构和工艺，有效解决了硫系玻璃现有技术熔炼效率低、组成性能一致性控制难度大等问题，可很好地实现高质量硫系玻璃的高效熔炼和批量制备，进一步提高红外玻璃的实用化水平，从而更加适于实用。The main purpose of the present invention is to provide an induction melting equipment and melting method for chalcogenide infrared glass and the chalcogenide infrared glass prepared therefrom. Through the specially designed furnace body structure and process, the existing technology of chalcogenide glass is effectively solved Problems such as low smelting efficiency and difficulty in controlling the consistency of composition and performance can well realize the efficient smelting and batch preparation of high-quality chalcogenide glass, and further improve the practical level of infrared glass, making it more suitable for practical use.
本发明的目的及解决其技术问题是采用以下技术方案来实现的。The purpose of the present invention and the solution to its technical problems are achieved by adopting the following technical solutions.
依据本发明提出的一种硫系玻璃的制备装置，包括，熔化模块、升降模块、均化模块、冷却模块、传送模块和坩埚，其中，所述的熔化模块包括炉盖、炉体、中频感应线圈和感应发热体，所述的炉盖和炉体构成熔化腔体，所述的熔化腔体底部开口，所述的中频感应线圈位于所述的熔化腔体内，所述的中频感应线圈使所述的感应发热体升温；所述的升降模块包括升降杆和升降控制系统，所述的升降模块用于带动所述的坩埚做第一运动；所述的均化模块包括保温炉和温度控制系统；所述的传送模块包括传送带和速度控制系统，所述的传送模块用于带动所述的坩埚做第二运动。A preparation device for chalcogenide glass according to the present invention includes a melting module, a lifting module, a homogenizing module, a cooling module, a conveying module and a crucible, wherein the melting module includes a furnace cover, a furnace body, an intermediate frequency induction Coil and induction heating element, the furnace cover and the furnace body constitute a melting cavity, the bottom of the melting cavity is open, the intermediate frequency induction coil is located in the melting cavity, and the intermediate frequency induction coil makes the melting cavity The temperature of the induction heating element is raised; the lifting module includes a lifting rod and a lifting control system, and the lifting module is used to drive the crucible to perform the first movement; the homogenization module includes a holding furnace and a temperature control system ; The transfer module includes a conveyor belt and a speed control system, and the transfer module is used to drive the crucible to make a second movement.
本发明的目的及解决其技术问题还可采用以下技术措施进一步实现。The purpose of the present invention and its technical problems can also be further realized by adopting the following technical measures.
优选的，前述的一种硫系玻璃的制备装置，其中所述的中频感应线圈由铜质空心金属管缠绕而成，线圈内通有冷却循环水。Preferably, the aforementioned device for preparing chalcogenide glass, wherein the intermediate frequency induction coil is wound by a copper hollow metal tube, and cooling circulating water is passed through the coil.
优选的，前述的一种硫系玻璃的制备装置，其中所述的感应发热体的材质为金属。Preferably, in the aforementioned device for preparing chalcogenide glass, the material of the induction heating element is metal.
优选的，前述的一种硫系玻璃的制备装置，其中所述的感应发热体的材质为铂金、金或不锈钢。Preferably, in the aforementioned device for preparing chalcogenide glass, the material of the induction heating element is platinum, gold or stainless steel.
优选的，前述的一种硫系玻璃的制备装置，其中所述的坩埚的材质为脱羟石英玻璃。Preferably, in the aforementioned device for preparing chalcogenide glass, the material of the crucible is dehydroxylated quartz glass.
优选的，前述的一种硫系玻璃的制备装置，其中所述的制备装置还包括机械卡钳，所述的机械卡钳用于移动所述的坩埚。Preferably, the aforementioned preparation device for chalcogenide glass, wherein the preparation device further includes a mechanical caliper, and the mechanical caliper is used to move the crucible.
优选的，前述的一种硫系玻璃的制备装置，其中所述的传送模块还包括保温层，所述的保温层铺设于所述的传送带上。Preferably, in the aforementioned device for preparing chalcogenide glass, the transmission module further includes an insulation layer, and the insulation layer is laid on the conveyor belt.
本发明的目的及解决其技术问题还采用以下的技术方案来实现。The purpose of the present invention and the solution to its technical problems are also achieved by the following technical solutions.
依据本发明提出的一种硫系玻璃的制备方法，根据上述任一项所述的一种硫系玻璃的制备装置，所述的制备方法包括，配料提纯：称量硫系玻璃原料，并加入除氧剂，得混合物料，将所述的混合物料装入第一坩埚中，其中，所述的原料的质量百分含量大于或等于99.999％，所述的原料的粒径为2-5mm，将装入混合物料后的第一坩埚抽真空，至第一坩埚内的真空度小于或等于10-3Pa，将所述的第一坩埚进行烘烤，以进行原料的纯化，纯化后，将第一坩埚进行真空熔封；熔化：将真空熔封后的第一坩埚放置在所述的升降杆上部，所述的升降模块将所述的第一坩埚送至感应发热体的空腔内，所述的中频感应线圈加热所述的感应发热体，所述的感应发热体将热量传导至第一坩埚，至第一坩埚内的原料的温度为800-950℃，加热时间为2-5h；均化：熔化完成后，所述的升降模块将所述的第一坩埚转移至均化模块，所述的传送模块带动所述的第一坩埚在均化模块内移动，并完成均化；冷却：均化后，传送模块将第一坩埚转移至冷却模块，进行冷却，至第一坩埚内的玻璃凝固成型，退火，得到硫系玻璃毛坯。According to the preparation method of a chalcogenide glass proposed in the present invention, according to the preparation device of a kind of chalcogenide glass described in any one of the above, the preparation method includes: purifying ingredients: weighing the chalcogenide glass raw materials, and adding Oxygen scavenger, to obtain a mixed material, put the mixed material into the first crucible, wherein the mass percentage of the raw material is greater than or equal to 99.999%, and the particle size of the raw material is 2-5mm, Vacuumize the first crucible filled with the mixed materials until the vacuum degree in the first crucible is less than or equal to 10 -3 Pa, and bake the first crucible to purify the raw materials. After the purification, the The first crucible is vacuum-sealed; melting: the first crucible after vacuum-sealed is placed on the upper part of the lifting rod, and the lifting module sends the first crucible to the cavity of the induction heating element, The induction heating element is heated by the intermediate frequency induction coil, and the induction heating element conducts heat to the first crucible, the temperature of the raw material in the first crucible is 800-950°C, and the heating time is 2-5h; Homogenization: After the melting is completed, the lifting module transfers the first crucible to the homogenization module, and the transfer module drives the first crucible to move in the homogenization module to complete the homogenization; cooling : After homogenization, the transfer module transfers the first crucible to the cooling module for cooling until the glass in the first crucible is solidified and formed, and annealed to obtain a chalcogenide glass blank.
本发明的目的及解决其技术问题还可采用以下技术措施进一步实现。The purpose of the present invention and its technical problems can also be further realized by adopting the following technical measures.
优选的，前述的一种硫系玻璃的制备方法，所述的第一坩埚熔化完成，将所述的第一坩埚转移至均化模块后，将第二坩埚送至感应发热体的空腔内进行熔化，并将所述的第一坩埚与所述的第二坩埚一同退火，所述的第二坩埚的混合物料，以及抽真空和真空封熔过程与第一坩埚相同。Preferably, in the aforementioned method for preparing chalcogenide glass, the melting of the first crucible is completed, and after the first crucible is transferred to the homogenization module, the second crucible is sent to the cavity of the induction heating element Melting is carried out, and the first crucible and the second crucible are annealed together, and the mixing materials of the second crucible, as well as the process of vacuuming and vacuum sealing are the same as those of the first crucible.
优选的，前述的一种硫系玻璃的制备方法，其中所述的均化的均化温度为400-600℃，均化时间为30-60分钟；所述冷却的冷却温度为280-350℃，冷却时间为2-5分钟。Preferably, the aforementioned method for preparing chalcogenide glass, wherein the homogenization temperature of the homogenization is 400-600°C, and the homogenization time is 30-60 minutes; the cooling temperature of the cooling is 280-350°C , the cooling time is 2-5 minutes.
本发明的目的及解决其技术问题还采用以下的技术方案来实现。The purpose of the present invention and the solution to its technical problems are also achieved by the following technical solutions.
依据本发明提出的一种硫系玻璃，所述的硫系玻璃由上述任一项的硫系玻璃的制备方法制备而得。According to the chalcogenide glass proposed in the present invention, the chalcogenide glass is prepared by any one of the above-mentioned chalcogenide glass preparation methods.
借由上述技术方案，本发明硫系玻璃及其制备方法和装置，至少具有下列优点：With the above technical solution, the chalcogenide glass and its preparation method and device of the present invention have at least the following advantages:
1、本发明采用感应加热方式，熔炼温度高、速度快、效率高，相比现有摇摆熔炼设备，生产效率提高一倍以上(现在硫系玻璃每炉次熔炼时间约为60-80小时，本方法可缩短为10-20小时，且可实现连续式生产，效率大大提高)；另外由于感应加热形成梯度温场，玻璃液会产生强烈的电磁扰动及温差对流，起到高速搅拌作用，有利于玻璃的充分反应和均化，有效消除分相、结石等缺陷，提高玻璃的熔化效率和组成均匀性。1. The present invention adopts the induction heating method, which has high smelting temperature, fast speed and high efficiency. Compared with the existing swing smelting equipment, the production efficiency is more than doubled (currently, the smelting time of each furnace of chalcogenide glass is about 60-80 hours, This method can be shortened to 10-20 hours, and continuous production can be realized, and the efficiency is greatly improved); in addition, due to the formation of a gradient temperature field by induction heating, the glass liquid will generate strong electromagnetic disturbance and temperature difference convection, which will play a role in high-speed stirring, which is effective It is beneficial to the full reaction and homogenization of the glass, effectively eliminates defects such as phase separation and stone formation, and improves the melting efficiency and composition uniformity of the glass.
2、本发明在真空密闭容器中提纯、熔化和冷却成型。各组分原料充分反应形成玻璃，有效减少了原料挥发，保证了硫系玻璃的组成和性能一致性，避免了不同炉次之间的性能波动，产品质量的批次稳定性好，有利于产品的批量化应用。2. The present invention is purified, melted and cooled in a vacuum-tight container. The raw materials of each component are fully reacted to form glass, which effectively reduces the volatilization of raw materials, ensures the composition and performance consistency of chalcogenide glass, avoids performance fluctuations between different furnaces, and has good batch stability of product quality, which is conducive to product quality. batch applications.
3、本发明不采用摇摆熔化方式，对石英坩埚的震动小，所以在设备空间允许条件下，坩埚规格尺寸可随意设计变更，可实现较大或特殊尺寸规格硫系玻璃制品的熔炼和制备。3. The present invention does not adopt the rocking melting method, and the vibration of the quartz crucible is small. Therefore, under the condition of equipment space, the size of the crucible can be designed and changed at will, and the melting and preparation of chalcogenide glass products with larger or special sizes can be realized.
4、本发明中，硫系玻璃的熔化、均化、退火过程可实现连续批次作业，熔化效率、批量生产能力大幅提高，日产能力可超过100公斤。4. In the present invention, the melting, homogenizing and annealing processes of chalcogenide glass can realize continuous batch operation, the melting efficiency and batch production capacity are greatly improved, and the daily production capacity can exceed 100 kg.
5、本发明的熔炼设备不需要真空炉、摇摆机构、气氛保护等设施保障，设备寿命长、工艺实现简单、生产成本低。5. The smelting equipment of the present invention does not require facilities such as a vacuum furnace, a swing mechanism, and atmosphere protection. The equipment has a long service life, simple process implementation, and low production costs.
上述说明仅是本发明技术方案的概述，为了能够更清楚了解本发明的技术手段，并可依照说明书的内容予以实施，以下以本发明的较佳实施例并配合附图详细说明如后。The above description is only an overview of the technical solutions of the present invention. In order to understand the technical means of the present invention more clearly and implement them according to the contents of the description, the preferred embodiments of the present invention and accompanying drawings are described in detail below.
附图说明Description of drawings
图1是本发明实施例提供的一种硫系红外玻璃感应熔炼装置示意图。Fig. 1 is a schematic diagram of a chalcogenide infrared glass induction melting device provided by an embodiment of the present invention.
其中，熔化模块A，升降模块B，均化模块C，冷却模块D，传送模块E，炉盖1，炉体2，中频感应线圈3，坩埚4，感应发热体5，升降杆6，机械卡钳7，保温炉8，吹风嘴9，传送带10，保温层11。Among them, melting module A, lifting module B, homogenizing module C, cooling module D, transmission module E, furnace cover 1, furnace body 2, intermediate frequency induction coil 3, crucible 4, induction heating element 5, lifting rod 6, mechanical calipers 7. Holding furnace 8, blowing nozzle 9, conveyor belt 10, insulation layer 11.
图2(a)是本发明实施例制得硫系玻璃的红外透射成像图，(b)是本发明对比例制得硫系玻璃的红外透射成像图。Fig. 2 (a) is an infrared transmission imaging diagram of the chalcogenide glass prepared in the embodiment of the present invention, and (b) is an infrared transmission imaging diagram of the chalcogenide glass prepared in the comparative example of the present invention.
具体实施方式detailed description
为更进一步阐述本发明为达成预定发明目的所采取的技术手段及功效，以下结合附图及较佳实施例，对依据本发明提出的一种硫系玻璃及其制备方法和装置，其具体实施方式、结构、特征及其功效，详细说明如后。在下述说明中，不同的“一实施例”或“实施例”指的不一定是同一实施例。此外，一或多个实施例中的特定特征、结构或特点可由任何合适形式组合。In order to further explain the technical means and effects adopted by the present invention to achieve the intended invention purpose, the specific implementation of a chalcogenide glass and its preparation method and device proposed according to the present invention will be described below in conjunction with the accompanying drawings and preferred embodiments. Mode, structure, feature and effect thereof are as follows in detail. In the following description, different "one embodiment" or "embodiment" do not necessarily refer to the same embodiment. Furthermore, the particular features, structures or characteristics of one or more embodiments may be combined in any suitable manner.
本发明提供一种硫系玻璃的制备装置，包括，熔化模块、升降模块、均化模块、冷却模块、传送模块和坩埚，其中，所述的熔化模块包括炉盖、炉体、中频感应线圈和感应发热体，所述的炉盖和炉体构成熔化腔体，所述的熔化腔体底部开口，所述的中频感应线圈位于所述的熔化腔体内，所述的中频感应线圈使所述的感应发热体升温；所述的升降模块包括升降杆和升降控制系统，所述的升降模块用于带动所述的坩埚做第一运动；所述的均化模块包括保温炉和温度控制系统；所述的传送模块包括传送带和速度控制系统，所述的传送模块用于带动所述的坩埚做第二运动。The present invention provides a preparation device for chalcogenide glass, including a melting module, a lifting module, a homogenizing module, a cooling module, a transmission module and a crucible, wherein the melting module includes a furnace cover, a furnace body, an intermediate frequency induction coil and Induction heating element, the furnace cover and the furnace body constitute a melting cavity, the bottom of the melting cavity is open, the intermediate frequency induction coil is located in the melting cavity, and the intermediate frequency induction coil makes the The heating element is heated by induction; the lifting module includes a lifting rod and a lifting control system, and the lifting module is used to drive the crucible to perform the first movement; the homogenizing module includes a holding furnace and a temperature control system; The transmission module includes a conveyor belt and a speed control system, and the transmission module is used to drive the crucible to perform the second movement.
(1)本发明提供的硫系玻璃的制备装置，所述的中频感应线圈和感应发热体均位于所述的熔化腔体内。所述的感应线圈缠绕于所述的发热体外部，电流通过所述的中频感应线圈产生感应磁场，磁场再作用于感应发热体产生电流而发热。所述的中频感应线圈不与所述的感应发热体接触，与感应发热体之间有一定的距离。此处的距离优选为：20-40mm。本发明中，由于中频感应线圈的中间、两端磁场密度不同，所以对感应发热体产生的电流强度不同，感应发热体中间部位温度最高，两端较弱，就产生温度梯度。(2)优选的，所述的第一运动为垂直方向的运动，所述的第二运动为水平方向的运动。(3)优选的，所述的炉盖和炉体均由耐火保温材料构成。(4)优选的，所述升降杆包括圆柱形杆和顶部托盘，所述的圆柱形杆为不锈钢材质，所述的顶部托盘可采用石英玻璃或耐热不锈钢材料，顶部托盘起到承载坩埚及封盖熔化部腔体作用。(5)优选的，所述的均化部为隧道式保温炉构成，采用电阻丝加热，并通过K型热电偶进行温度测量和控制。(6)硫系玻璃熔液经均化后，由传送带牵引出玻璃均化部，在冷却成形部通过多个吹风嘴以风冷方式进行快速冷却，使玻璃凝固成形。(1) In the preparation device for chalcogenide glass provided by the present invention, both the intermediate frequency induction coil and the induction heating element are located in the melting cavity. The induction coil is wound outside the heating element, the current passes through the intermediate frequency induction coil to generate an induction magnetic field, and the magnetic field acts on the induction heating element to generate current and generate heat. The intermediate frequency induction coil is not in contact with the induction heating body, and has a certain distance from the induction heating body. The distance here is preferably: 20-40mm. In the present invention, due to the different magnetic field densities at the middle and both ends of the intermediate frequency induction coil, the current intensities generated on the induction heating element are different. The temperature in the middle of the induction heating element is the highest and the two ends are weaker, thus generating a temperature gradient. (2) Preferably, the first movement is a movement in the vertical direction, and the second movement is a movement in the horizontal direction. (3) Preferably, both the furnace cover and the furnace body are made of refractory and heat-insulating materials. (4) Preferably, the lifting rod includes a cylindrical rod and a top tray, the cylindrical rod is made of stainless steel, the top tray can be made of quartz glass or heat-resistant stainless steel, and the top tray acts as a bearing crucible and Capping the cavity of the melting part. (5) Preferably, the homogenization part is composed of a tunnel-type holding furnace, which is heated by resistance wire, and the temperature is measured and controlled by a K-type thermocouple. (6) After the chalcogenide glass melt is homogenized, it is pulled out of the glass homogenization section by the conveyor belt, and is rapidly cooled by air cooling through multiple blowing nozzles in the cooling forming section, so that the glass is solidified and formed.
优选的，所述的中频感应线圈由铜质空心金属管缠绕而成，线圈内通有冷却循环水。Preferably, the intermediate frequency induction coil is wound by a copper hollow metal tube, and cooling circulating water is passed through the coil.
优选的，所述的感应发热体的材质为金属；所述的感应发热体的结构为中空的圆筒结构，所述的感应发热体的底部有开口。优选的，所述的发热体的厚度为2-10mm，所述的感应发热体为圆筒状结构，发热效率高。所述的感应发热体的下部有开口，以利于坩埚的升降。当坩埚置于熔化部时，所述的感应发热体与所述坩埚之间的距离大于或等于5mm，优选的，所述的距离为5-10mm，该距离即可以保证坩埚可以顺利的进行上下移动，也有利于感应发热体将热量传递给坩埚。Preferably, the material of the induction heating element is metal; the structure of the induction heating element is a hollow cylindrical structure, and the bottom of the induction heating element has an opening. Preferably, the thickness of the heating element is 2-10mm, and the induction heating element has a cylindrical structure with high heating efficiency. The lower part of the induction heating element has an opening to facilitate the lifting of the crucible. When the crucible is placed in the melting part, the distance between the induction heating element and the crucible is greater than or equal to 5mm, preferably, the distance is 5-10mm, which can ensure that the crucible can go up and down smoothly The movement is also beneficial to the induction heating element to transfer heat to the crucible.
优选的，所述的感应发热体的材质为空气中耐高温、抗氧化的材料，例如，铂金、金等贵金属，以及耐热不锈钢。优选的，所述的不锈钢为0Cr25Ni20、1Cr18Ni9Ti或0Cr23Ni13等。Preferably, the material of the induction heating element is a material that is resistant to high temperature and oxidation in the air, such as precious metals such as platinum and gold, and heat-resistant stainless steel. Preferably, the stainless steel is 0Cr25Ni20, 1Cr18Ni9Ti or 0Cr23Ni13, etc.
优选的，所述的坩埚的材质为脱羟石英玻璃。Preferably, the material of the crucible is dehydroxylated quartz glass.
本发明中坩埚的材质优选为脱羟石英玻璃。相对于普通石英玻璃，脱羟石英玻璃中没有氢氧根，在高温下不会释放出氧气，有利于提高制备得到的硫系玻璃的纯度。The material of the crucible in the present invention is preferably dehydroxylated quartz glass. Compared with ordinary quartz glass, there is no hydroxide in dehydroxylated quartz glass, and oxygen will not be released at high temperature, which is beneficial to improve the purity of the prepared chalcogenide glass.
优选的，所述的制备装置还包括机械卡钳，所述的机械卡钳用于移动所述的坩埚。Preferably, the preparation device further includes a mechanical caliper, and the mechanical caliper is used to move the crucible.
所述的机械卡钳可实现抓取坩埚，并将坩埚移动至均化部的功能。The mechanical caliper can realize the function of grabbing the crucible and moving the crucible to the homogenization part.
优选的，所述的传送模块还包括保温层，所述的保温层铺设于所述的传送带上。Preferably, the transfer module further includes an insulation layer, and the insulation layer is laid on the conveyor belt.
此处的“所述的保温层铺设于所述的传送带上”，是指，所述的保温层与所述的传送带接触，这里的“上”并非“上部”，不做任何位置关系的限定。例如，所述的保温层可以位于传送带的上部，也可以位于传送带的下部。Here, "the insulation layer is laid on the conveyor belt" means that the insulation layer is in contact with the conveyor belt, and the "upper" here is not the "upper part", and there is no limitation on the positional relationship. . For example, the thermal insulation layer can be located on the upper part of the conveyor belt, or on the lower part of the conveyor belt.
(1)优选的，所述的传送带通过所述的均化部的底部，带动所述的坩埚通过所述的隧道式保温炉，达到保温均化的作用。(2)优选的，所述的传送带采用Ni80Cr20等耐热不锈钢丝编制而成，构成平整、耐高温传动传送带；优选的，所述的保温层铺设于所述的传送带的下部，保温层采用电阻丝的加热方式对传送带进行加热保温。(1) Preferably, the conveyor belt passes through the bottom of the homogenization section, and drives the crucible through the tunnel-type holding furnace to achieve heat preservation and homogenization. (2) Preferably, the conveyor belt is made of heat-resistant stainless steel wire such as Ni80Cr20 to form a flat, high-temperature-resistant transmission conveyor belt; preferably, the thermal insulation layer is laid on the lower part of the conveyor belt, and the thermal insulation layer adopts electric resistance The heating method of the wire is used to heat and keep the conveyor belt warm.
本发明进一步提供了一种硫系玻璃的制备方法。The invention further provides a preparation method of chalcogenide glass.
配料提纯：称量硫系玻璃原料，并加入除氧剂，得混合物料，将所述的混合物料装入第一坩埚中，其中，所述的原料的质量百分含量大于或等于99.999％，所述的原料的粒径为2-5mm，将装入混合物料后的第一坩埚抽真空，至第一坩埚内的真空度小于或等于10-3Pa，将所述的第一坩埚进行烘烤，以进行原料的纯化，纯化后，将第一坩埚进行真空熔封。熔化：将真空熔封后的第一坩埚放置在所述的升降杆上部，所述的升降模块将所述的第一坩埚送至感应发热体的空腔内，所述的中频感应线圈加热所述的感应发热体，所述的感应发热体将热量传导至第一坩埚，至第一坩埚内的原料的温度为800-950℃(此处的原料，为第一坩埚内的物料，当原料处于此温度下时，固态的原料熔化为玻璃液，所以，此时的原料为此温度下的玻璃液)，加热时间为2-5h。均化：熔化完成后，所述的升降模块将所述的第一坩埚转移至均化模块，所述的传送模块带动所述的第一坩埚在均化模块内移动，并完成均化。冷却：均化后，传送模块将第一坩埚转移至冷却模块，进行冷却，至第一坩埚内的玻璃凝固成型，退火，得到硫系玻璃。Purification of ingredients: weighing chalcogenide glass raw materials, and adding oxygen scavenger to obtain a mixed material, and putting the mixed material into the first crucible, wherein the mass percentage of the raw material is greater than or equal to 99.999%, The particle size of the raw material is 2-5 mm, and the first crucible loaded with the mixed material is vacuumized until the vacuum degree in the first crucible is less than or equal to 10 -3 Pa, and the first crucible is baked To purify the raw materials, after the purification, the first crucible is vacuum-sealed. Melting: place the vacuum-sealed first crucible on the upper part of the lifting rod, the lifting module sends the first crucible to the cavity of the induction heating element, and the intermediate frequency induction coil heats the The above induction heating element, the induction heating element conducts heat to the first crucible, and the temperature of the raw material in the first crucible is 800-950°C (the raw material here is the material in the first crucible, when the raw material When at this temperature, the solid raw material melts into molten glass, so the raw material at this time is molten glass at this temperature), and the heating time is 2-5 hours. Homogenization: After the melting is completed, the lifting module transfers the first crucible to the homogenization module, and the transfer module drives the first crucible to move in the homogenization module to complete the homogenization. Cooling: After homogenization, the transfer module transfers the first crucible to the cooling module for cooling until the glass in the first crucible is solidified and formed, annealed to obtain chalcogenide glass.
感应加热下，玻璃液体由于热量传导、对流会产生流动，这样内部会出现条纹，本发明所述的均化过程，使得玻璃液稳定均匀，消除流动条纹。Under induction heating, the glass liquid will flow due to heat conduction and convection, so that streaks will appear inside. The homogenization process described in the present invention makes the glass liquid stable and uniform, eliminating flow streaks.
优选的，所述的除氧剂为高纯的金属铝。Preferably, the oxygen scavenger is high-purity metal aluminum.
优选的，所述的第一坩埚熔化完成，将所述的第一坩埚转移至均化模块后，将第二坩埚送至感应发热体的空腔内进行熔化，并将所述的第一坩埚与所述的第二坩埚一同退火，所述的第二坩埚的混合物料，以及抽真空和真空封熔过程与第一坩埚相同。Preferably, the melting of the first crucible is completed. After the first crucible is transferred to the homogenization module, the second crucible is sent to the cavity of the induction heating element for melting, and the first crucible is It is annealed together with the second crucible, and the mixed materials of the second crucible, as well as the process of vacuuming and vacuum sealing are the same as those of the first crucible.
优选的，根据硫系玻璃成分、料量的差异不同，所述均化的均化温度为400-600℃，均化时间为30-60分钟；所述冷却的冷却温度为280-350℃，冷却时间为2-5分钟。Preferably, according to the differences in chalcogenide glass components and material amounts, the homogenization temperature of the homogenization is 400-600°C, and the homogenization time is 30-60 minutes; the cooling temperature of the cooling is 280-350°C, The cooling time is 2-5 minutes.
实施例Example
本实施例提供了一种利用本发明提供的硫系玻璃的制备装置制备硫系玻璃的过程。硫系玻璃的制备装置如图1所示。This embodiment provides a process for preparing chalcogenide glass using the device for preparing chalcogenide glass provided by the present invention. The preparation device of chalcogenide glass is shown in Fig. 1 .
配料提纯：按照设计比例，在厌氧、厌水手套箱内分别称量所需的硫系玻璃原料，和除氧剂混合后形成配合料，装入石英玻璃坩埚4中。所用原料纯度优于99.999％，材料粒径2～5mm。本实施例中，原料的质量为2公斤，坩埚的体积为1.5升。Purification of ingredients: According to the design ratio, the required chalcogenide glass raw materials are weighed in the anaerobic and anaerobic glove boxes, mixed with the oxygen scavenger to form a batch, and loaded into the quartz glass crucible 4 . The purity of the raw materials used is better than 99.999%, and the particle size of the material is 2-5mm. In this embodiment, the quality of the raw material is 2 kg, and the volume of the crucible is 1.5 liters.
将所述石英玻璃坩埚抽真空，真空度不大于10-3Pa，然后将抽真空的石英玻璃坩埚在200～400℃下进行烘烤3～10小时进行原料纯化。纯化完成后用氢氧焰对石英玻璃坩埚4进行真空熔封。Vacuum the quartz glass crucible to a degree of no more than 10 -3 Pa, then bake the vacuumed quartz glass crucible at 200-400° C. for 3-10 hours to purify the raw material. After the purification is completed, the quartz glass crucible 4 is vacuum-sealed with an oxyhydrogen flame.
玻璃熔化：将真空熔封好的石英玻璃坩埚放置在升降杆6上部，开启升降机构B将坩埚送入熔化部A的由炉盖1、炉体2、中频感应线圈3和感应发热体5所形成的熔化腔体内。启动电源，中频感应线圈驱动感应发热体5发热，加热石英玻璃坩埚中的玻璃，升温速度10～20℃/min，可在1～2小时内快速达到硫系玻璃的熔化温度(一般800～950℃)。本实施例中，中频感应线圈的缠绕方式为环形缠绕，匝数为10、口径为240mm。Glass melting: Place the vacuum-sealed quartz glass crucible on the upper part of the lifting rod 6, open the lifting mechanism B to send the crucible into the melting part A, which is composed of furnace cover 1, furnace body 2, intermediate frequency induction coil 3 and induction heating element 5 In the formed melting cavity. Turn on the power supply, the intermediate frequency induction coil drives the induction heating element 5 to generate heat, and heats the glass in the quartz glass crucible. The heating rate is 10-20°C/min, and the melting temperature of the chalcogenide glass can be quickly reached within 1-2 hours (generally 800-950 ℃). In this embodiment, the winding mode of the intermediate frequency induction coil is circular winding, the number of turns is 10, and the diameter is 240 mm.
在熔化温度下熔化2～5小时可完成硫系玻璃的熔化过程(传统摇摆法的熔化时间一般都在10小时以上)。Melting at the melting temperature for 2 to 5 hours can complete the melting process of the chalcogenide glass (the melting time of the traditional rocking method is generally more than 10 hours).
玻璃均化：完成熔化过程后，开启升降机构B，升降杆6下降，将石英玻璃坩埚移出熔化部，降至均化工位，操纵机械卡钳7夹取坩埚后，将坩埚平稳移至玻璃均化部C中的传送带10上，传送带10的下部铺设有保温层11。Glass homogenization: After the melting process is completed, the lifting mechanism B is opened, the lifting rod 6 is lowered, the quartz glass crucible is moved out of the melting part, and lowered to the homogenization position. On the conveyor belt 10 in part C, the lower part of the conveyor belt 10 is laid with an insulating layer 11 .
传送带10牵引坩埚在隧道式保温炉8中平稳缓慢移动，在设定的均化温度、时间内通过玻璃均化部C，完成过程。The conveyor belt 10 pulls the crucible to move steadily and slowly in the tunnel-type holding furnace 8, and passes through the glass homogenization part C within the set homogenization temperature and time to complete the process.
风冷成形：硫系玻璃均化后进入冷却成形部D进行快速风冷降温、凝固成形。Air-cooled forming: after homogenization, the chalcogenide glass enters the cooling and forming section D for rapid air-cooling and cooling, solidification and forming.
石英玻璃坩埚在传送带10牵引下缓慢通过冷却成形部D，开启压缩空气送风装置，压缩空气通过多个吹风嘴9对石英玻璃坩埚进行快速吹风降温，使得硫系玻璃熔液迅速冷却至凝固成形温度。The quartz glass crucible slowly passes through the cooling forming part D under the traction of the conveyor belt 10, and the compressed air blowing device is turned on, and the compressed air passes through a plurality of blowing nozzles 9 to quickly blow and cool the quartz glass crucible, so that the chalcogenide glass melt is rapidly cooled to solidification and forming temperature.
在设定冷却时间、风速下完成硫系玻璃的成形，成形后坩埚可迅速移至专用退火炉中，经退火降温后可得到硫系玻璃毛坯。The forming of chalcogenide glass is completed under the set cooling time and wind speed. After forming, the crucible can be quickly moved to the special annealing furnace, and the chalcogenide glass blank can be obtained after annealing and cooling.
上述工艺流程中，硫系玻璃完成熔化，移入玻璃均化部C后，可继续将真空封装好的坩埚由升降装置B送入熔化部A开始新一炉次的熔炼过程；风冷成形后的多埚硫系玻璃可在退火炉中统一进行退火。通过上述工艺过程，可以实现硫系玻璃的连续感应熔炼过程。In the above process flow, after the chalcogenide glass is melted and moved into the glass homogenization part C, the vacuum-packaged crucible can be sent to the melting part A by the lifting device B to start a new melting process; Multi-pot chalcogenide glasses can be uniformly annealed in an annealing furnace. Through the above process, the continuous induction melting process of chalcogenide glass can be realized.
图2(a)为本实施例制得硫系玻璃的红外透射成像图(成像波长1.5μm)。Fig. 2(a) is an infrared transmission imaging image (imaging wavelength 1.5 μm) of the chalcogenide glass prepared in this example.
经检测，本实施例制得的硫系玻璃批次稳定性可达到(Δn)1×10-3以下。After testing, the batch stability of the chalcogenide glass prepared in this example can reach below (Δn)1×10 -3 .
对比例comparative example
采用传统摇摆法的制备上述实施例中的硫系玻璃。The chalcogenide glasses in the above examples were prepared by the traditional rocking method.
图2(b)为本对比例制得硫系玻璃的红外透射成像图(成像波长1.5μm)。Fig. 2(b) is an infrared transmission imaging image (imaging wavelength 1.5 μm) of the chalcogenide glass prepared in this comparative example.
在上述实施例中，对各个实施例的描述都各有侧重，某个实施例中没有详述的部分，可以参见其他实施例的相关描述。In the foregoing embodiments, the descriptions of each embodiment have their own emphases, and for parts not described in detail in a certain embodiment, reference may be made to relevant descriptions of other embodiments.
可以理解的是，上述装置中的相关特征可以相互参考。另外，上述实施例中的“第一”、“第二”等是用于区分各实施例，而并不代表各实施例的优劣。It can be understood that related features in the above devices can refer to each other. In addition, "first", "second" and so on in the above embodiments are used to distinguish each embodiment, and do not represent the advantages and disadvantages of each embodiment.
在此处所提供的说明书中，说明了大量具体细节。然而，能够理解，本发明的实施例可以在没有这些具体细节的情况下实践。在一些实例中，并未详细示出公知的结构和技术，以便不模糊对本说明书的理解。In the description provided herein, numerous specific details are set forth. However, it is understood that embodiments of the invention may be practiced without these specific details. In some instances, well-known structures and techniques have not been shown in detail in order not to obscure the understanding of this description.
类似地，应当理解，为了精简本公开并帮助理解各个发明方面中的一个或多个，在上面对本发明的示例性实施例的描述中，本发明的各个特征有时被一起分组到单个实施例、图、或者对其的描述中。然而，并不应将该公开的装置解释成反映如下意图：即所要求保护的本发明要求比在每个权利要求中所明确记载的特征更多的特征。更确切地说，如下面的权利要求书所反映的那样，发明方面在于少于前面公开的单个实施例的所有特征。因此，遵循具体实施方式的权利要求书由此明确地并入该具体实施方式，其中每个权利要求本身都作为本发明的单独实施例。Similarly, it should be appreciated that in the foregoing description of exemplary embodiments of the invention, in order to streamline this disclosure and to facilitate an understanding of one or more of the various inventive aspects, various features of the invention are sometimes grouped together in a single embodiment, figure, or its description. This disclosed device, however, is not to be interpreted as reflecting an intention that the claimed invention requires more features than are expressly recited in each claim. Rather, as the following claims reflect, inventive aspects lie in less than all features of a single foregoing disclosed embodiment. Thus, the claims following the Detailed Description are hereby expressly incorporated into this Detailed Description, with each claim standing on its own as a separate embodiment of this invention.
本领域那些技术人员可以理解，可以对实施例中的装置中的部件进行自适应性地改变并且把它们设置在与该实施例不同的一个或多个装置中。可以把实施例中的部件组合成一个部件，以及此外可以把它们分成多个子部件。除了这样的特征中的至少一些是相互排斥之外，可以采用任何组合对本说明书(包括伴随的权利要求、摘要和附图)中公开的所有特征以及如此公开的任何装置的所有部件进行组合。除非另外明确陈述，本说明书(包括伴随的权利要求、摘要和附图)中公开的每个特征可以由提供相同、等同或相似目的的替代特征来代替。Those skilled in the art can understand that the components in the device in the embodiment can be adaptively changed and arranged in one or more devices different from the embodiment. The components in the embodiments may be combined into one component, and furthermore may be divided into a plurality of subcomponents. All features disclosed in this specification (including accompanying claims, abstract and drawings) and all parts of any apparatus so disclosed may be combined in any combination, unless at least some of such features are mutually exclusive. Each feature disclosed in this specification (including accompanying claims, abstract and drawings) may be replaced by alternative features serving the same, equivalent or similar purpose, unless expressly stated otherwise.
此外，本领域的技术人员能够理解，尽管在此所述的一些实施例包括其它实施例中所包括的某些特征而不是其它特征，但是不同实施例的特征的组合意味着处于本发明的范围之内并且形成不同的实施例。例如，在下面的权利要求书中，所要求保护的实施例的任意之一都可以以任意的组合方式来使用。本发明的各个部件实施例可以以硬件实现，或者以它们的组合实现。Furthermore, those skilled in the art will understand that although some embodiments described herein include some features included in other embodiments but not others, combinations of features from different embodiments are meant to be within the scope of the invention. and form different embodiments. For example, in the following claims, any of the claimed embodiments may be used in any combination. The various component embodiments of the present invention can be implemented in hardware, or in a combination thereof.
应该注意的是上述实施例对本发明进行说明而不是对本发明进行限制，并且本领域技术人员在不脱离所附权利要求的范围的情况下可设计出替换实施例。在权利要求中，不应将位于括号之间的任何参考符号构造成对权利要求的限制。单词“包含”不排除存在未列在权利要求中的部件或组件。位于部件或组件之前的单词“一”或“一个”不排除存在多个这样的部件或组件。本发明可以借助于包括有若干不同部件的装置来实现。在列举了若干部件的权利要求中，这些部件中的若干个可以是通过同一个部件项来具体体现。单词第一、第二、以及第三等的使用不表示任何顺序。可将这些单词解释为名称。It should be noted that the above-mentioned embodiments illustrate rather than limit the invention, and that those skilled in the art will be able to design alternative embodiments without departing from the scope of the appended claims. In the claims, any reference signs placed between parentheses shall not be construed as limiting the claim. The word "comprising" does not exclude the presence of parts or components not listed in a claim. The word "a" or "an" preceding an element or component does not exclude the presence of a plurality of such elements or components. The invention can be implemented by means of an apparatus comprising several different components. In a claim enumerating several components, several of these components may be embodied by the same component item. The use of the words first, second, and third, etc. does not indicate any order. These words can be interpreted as names.
本发明中所述的数值范围包括此范围内所有的数值，并且包括此范围内任意两个数值组成的范围值。例如，“所述均化的均化温度为400-600℃”，此数值范围包括400-600之间所有的数值，并且包括此范围内任意两个数值(例如：450、500)组成的范围值(450-500)；本发明所有实施例中出现的同一指标的不同数值，可以任意组合，组成范围值。The numerical range stated in the present invention includes all the numerical values in this range, and includes the range value composed of any two numerical values in this range. For example, "the homogenization temperature of the homogenization is 400-600°C", this range of values includes all values between 400-600, and includes the range composed of any two values (for example: 450, 500) within this range Value (450-500); different numerical values of the same index appearing in all embodiments of the present invention can be combined arbitrarily to form a range value.
本发明权利要求和/或说明书中的技术特征可以进行组合，其组合方式不限于权利要求中通过引用关系得到的组合。通过权利要求和/或说明书中的技术特征进行组合得到的技术方案，也是本发明的保护范围。The technical features in the claims of the present invention and/or the description can be combined, and the combination is not limited to the combination obtained by reference in the claims. The technical solution obtained by combining the technical features in the claims and/or the description is also within the protection scope of the present invention.
以上所述，仅是本发明的较佳实施例而已，并非对本发明作任何形式上的限制，依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰，均仍属于本发明技术方案的范围内。The above are only preferred embodiments of the present invention, and are not intended to limit the present invention in any form. Any simple modifications, equivalent changes and modifications made to the above embodiments according to the technical essence of the present invention still belong to the present invention. within the scope of the technical solution of the invention.
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