CN103466933A - Extrusion device and method for extruding chalcogenide glass optical fiber perform with superposition method - Google Patents
Extrusion device and method for extruding chalcogenide glass optical fiber perform with superposition method Download PDFInfo
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- CN103466933A CN103466933A CN2013103641027A CN201310364102A CN103466933A CN 103466933 A CN103466933 A CN 103466933A CN 2013103641027 A CN2013103641027 A CN 2013103641027A CN 201310364102 A CN201310364102 A CN 201310364102A CN 103466933 A CN103466933 A CN 103466933A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/01265—Manufacture of preforms for drawing fibres or filaments starting entirely or partially from molten glass, e.g. by dipping a preform in a melt
- C03B37/01274—Manufacture of preforms for drawing fibres or filaments starting entirely or partially from molten glass, e.g. by dipping a preform in a melt by extrusion or drawing
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/80—Non-oxide glasses or glass-type compositions
- C03B2201/86—Chalcogenide glasses, i.e. S, Se or Te glasses
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- 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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Abstract
The invention discloses an extrusion device and method for extruding a chalcogenide glass optical fiber perform with a superposition method. A pushing mechanism of the extrusion device is arranged above an extrusion container, and an extrusion rod is fixedly connected with the pushing mechanism; a heating furnace set used for heating the extrusion container is arranged outside the extrusion container, and a vacuum chamber is arranged outside the heating furnace set and is connected with a vacuum pump; an extrusion pad is arranged in the extrusion container, and an extrusion outlet is formed in the lower end of the extrusion container; a mould is arranged at the bottom of the extrusion container, and a mould hole of the mould is communicated with the extrusion outlet; a heat reducing furnace used for annealing the extruded optical fiber perform is arranged at the bottom of the extrusion container, and a traction device is arranged at the lower part of the heat reducing furnace. The extrusion device and the method have the characteristics of good controllability and high production efficiency.; the superposition method is adopted to extrude chalcogenide glass, and the obtained optical fiber perform has uniform structural composition, smooth inner and outer surfaces and a perfect interface; a surface layer is provide with a protective layer composed of high-molecular polymers, so that a performance test after drawing optical fibers is facilitated.
Description
Technical field
The present invention relates to the preparation of chalcogenide glass fiber prefabricated rods, especially relate to squeezing device and method that a kind of superposition method extrudes the chalcogenide glass fiber prefabricated rods.
Background technology
In the telecommunication optical fiber preparation process, one of important content is the preparation of preform, traditional preform technology of preparing has four kinds of techniques at present, and these four kinds of techniques are respectively outer vapour deposition process (OVD), vapour phase axial deposition technique (VAD), improve vapour deposition process (MCVD) and plasma activated chemical vapour deposition technique (PCVD).Recent two decades comes, the OVD method develops into many blowtorch from single spraying lamp deposition and deposits simultaneously, sedimentation rate is multiplied, realize that an equipment deposits many rods, and the single stage method of making prefabricated rods from depositing successively the core covering develops into two step method simultaneously, first prepare large diameter plug, be drawn into again minor diameter plug or not drawing-down, then adopt the surrounding layer technology to prepare preform, improved production efficiency, reduced production cost.But MCVD method, especially PCVD method, OVD method and VAD method are more easily accurately controlled the radial refractive index distribution of plug, thereby for preparing multimode optical fibers MMF and non-zero dispersion fiber DZDF core prefabricated rods is more effective.
Chalcogenide glass has good mid and far infrared through performance, and specific refractory power is high, and has high nonlinear refraction rate coefficient etc.Due to its good infrared transmission performance, chalcogenide glass fiber can be applicable to mid-infrared laser Energy Transfer, space zero suppression interferometer, in the field such as infrared biological and chemical sensor, mid-infrared fiber laser.But the preparation method of the preform that above-mentioned OVD method, VAD method, MCVD method and PCVD method etc. are traditional, be not suitable for the preparation of chalcogenide glass fiber prefabricated rods.
Method of piling is the method for the current modal making chalcogenide glass fiber prefabricated rods of the invention such as the Monro of Southampton University of Southampton.2006, French Perfos company and French reyn 1 university combined a kind of baroque Ga that has reported prepared by the employing method of piling
5ge
20sb
10se
65microstructured optical fibers.Although method of piling is the current making method of ripe chalcogenide glass fiber prefabricated rods the most, but the method for piling workload is large, easily crisp chalcogenide glass tubule surface is prone to defect, and form kapillary inside that the kapillary boundling arranges in the heating drawing process and be prone to airport and subside and be out of shape, the defects such as the crystallization particle between the kapillary interface, bubble are also more, take gap between kapillary to merge the inadequate interfacial air defect generated as main in the process of subsiding.Because adopt the air pressure hierarchical control to be difficult to accurately control making and the wire drawing of many pores prefabricated rods of complex construction, so cause the chalcogenide glass microstructured optical fibers loss of preparation generally higher.
Casting is the preparation method of the another kind of chalcogenide glass fiber prefabricated rods of the invention of the people such as Quentin Coulombier by French reyn 1 university in 2010.Its process is roughly: in the silica tube of vacuum high-temperature sealing, the chalcogenide glass of the molten state after purifying is being flowed in many quartzy frame bodies of constructing with quartzy solid slim rods, be fixed on the quartzy thin slice of perforation before and after thin rod, in advance by the rear and quartzy tube wall bonding of oxyhydrogen flame heating for two quartzy thin slices, after high temperature is fully founded, silica tube is holded up, glass metal is flowed in the frame body of solid bar composition, fine annealing after quenching, the chalcogenide glass rod prepared is inserted to the hydrofluoric acid dips that concentration is 40%, quartzy thin rod is dissolved, thereby obtain the chalcogenide glass fiber prefabricated rods.With method of piling, compare, casting has clear superiority: such as casting technique is simple, avoided method of piling to pile up capillary glass tube and arranged the arrangement out of true that human factor causes, easily prepared the preform of different cross section structure etc.But, the chalcogenide glass fiber prefabricated rods prepared for casting, the chalcogenide glass microstructured optical fibers of follow-up preparation also has certain defect, can not prepare the different microstructured optical fibers of core covering component, and the smooth finish of corroding the hole inwall after inner quartz pushrod is still a key issue.
Although method of piling and casting have the case of successfully producing the chalcogenide glass fiber prefabricated rods, the fibre loss of producing due to these two kinds of methods is all very large, and the technique more complicated, is not suitable for large-scale production.Therefore be necessary the preparation method of the chalcogenide glass fiber prefabricated rods that exploitation makes new advances, improve quality and the production efficiency of chalcogenide glass fiber prefabricated rods.It is at present domestic that to prepare for superposition method patent and document that sulphur is preform less, wherein domestic patent CN1081654A is kind of a method of manufacturing preform, be mainly can obtain a kind ofly there is higher mechanical strength and do not have alveolate plastic optical fiber, rather than relate to the preparation of chalcogenide glass fiber prefabricated rods.What patent CN102531377 introduced is a kind of vacuum extruder for the preparation of the chalcogenide glass fiber prefabricated rods, extruding by extrusion machine to chalcogenide glass, make softening glass through mould, chalcogenide glass annealed processing again can obtain the chalcogenide glass fiber prefabricated rods, when but this extrusion machine extruding prepares the chalcogenide glass fiber prefabricated rods, its prefabricated rods of extruding is subject to the impact of gravity larger, cause the structure of prefabricated rods to form the various defects such as inhomogeneous, production efficiency is not high, and the quality of the optical fiber of follow-up drawing is had a negative impact.
Summary of the invention
Technical problem to be solved by this invention is: for the deficiencies in the prior art, provide a kind of controllability is good, production efficiency is high superposition method to extrude squeezing device and the method for chalcogenide glass fiber prefabricated rods.
The present invention solves the problems of the technologies described above adopted technical scheme: superposition method extrudes the squeezing device of chalcogenide glass fiber prefabricated rods, comprise pushing mechanism, extrusion stem, container, pressure pad and mould, described pushing mechanism is arranged on the top of described container, described extrusion stem is fixedly connected with described pushing mechanism, described container is outside equipped with the process furnace group for described container is heated, described process furnace group is outside equipped with vacuum chamber, described vacuum chamber is connected with vacuum pump, described pressure pad is arranged in described container, the lower end of described container is provided with extrusion, described mould is arranged on the bottom of described container, the nib of described mould is connected with described extrusion, the bottom of described container is provided with the stove of bringing down a fever of being annealed for the preform to extruding, the bottom of the described stove of bringing down a fever is provided with towing mechanism.
Preferably, described pressure pad is fixedly connected with described extrusion stem; Described bringing down a fever between stove and described towing mechanism is provided with for preventing from extruding the locating device that rod is crooked.Pressure pad is fixedly connected with extrusion stem, is convenient to the replacing of pressure pad, makes extrusion operation more convenient.
Preferably, described process furnace group comprises the first process furnace and the second process furnace, and described the first process furnace is arranged on the top of described container, and described the second process furnace is arranged on the bottom of described container.Different according to component and the compression properties of chalcogenide glass and high molecular polymer during use, set the temperature of different the first process furnace and the second process furnace, be conducive to carrying out smoothly of extrusion process.
Preferably, also comprise temperature control platform, the arranged outside of described container has temperature sensor, and described temperature sensor, described the first process furnace, described the second process furnace and the described stove of bringing down a fever are all controlled platform with described temperature and be connected.Temperature is controlled platform and can accurately be controlled the temperature of the first process furnace, the second process furnace and the stove of bringing down a fever, and has guaranteed accuracy and the controllability of temperature in extruding and the process of bringing down a fever.Simultaneous temperature is controlled the actual extrusion temperature of platform can be to extruding the time and is monitored, and when actual extrusion temperature surpasses the extrusion temperature of setting, temperature is controlled platform can automatic alarm.
Preferably, on described extrusion stem, pressure transmitter is installed, an end of described pressure transmitter is connected with a pressure-display device, and the other end of described pressure transmitter is connected with described pushing mechanism.Pressure transmitter and pressure-display device, can provide the squeeze size cases, is convenient to the management and control of extrusion process.
Preferably, described pushing mechanism is provided with pressure warning unit, and described pressure warning unit is connected with described pressure-display device.When the thrust of pushing mechanism, during higher than the squeeze set, pressure warning unit is reported to the police, and pushing mechanism quits work automatically.
Preferably, also comprise computer control platform, described computer is controlled platform and is connected with described temperature sensor with described pressure transmitter respectively.Computer is controlled platform can record squeeze and the time dependent data of extrusion temperature, has strengthened the controllability of extrusion process.
Preferably, the surface-coated of the internal surface of described container and described mould has graphite linings.Graphite has good thermotolerance, and in addition, after applying graphite linings on container and mould, the surface of the preform of extruding also can be attached with graphite, and the preform of extruding is had to certain provide protection.
Superposition method extrudes the method for chalcogenide glass fiber prefabricated rods, comprises the following steps:
1) be ready to chalcogenide glass and the high molecular polymer of polylith sheet, with alcohol, rinse post-drying, put into vacuum vessel;
2) at first take out a slice high molecular polymer, the chalcogenide glass of the polylith sheet that superposes successively on the top of this sheet high molecular polymer again, then the high molecular polymer after stack is put into to container together with chalcogenide glass, and make high molecular polymer be placed on the lowermost end of container;
3) utilize vacuum pump to vacuumize vacuum chamber, when the low vacuum of vacuum chamber in 10
-2during Pa, to topping up in vacuum chamber, make the air pressure in vacuum chamber identical with external atmosphere pressure;
4) open temperature and control platform, set the process furnace group and the temperature of stove of bringing down a fever, and the temperature T of setting mould is Tg<T<Tx, the recrystallization temperature that wherein Tx is chalcogenide glass, the transition temperature that Tg is chalcogenide glass makes the softening temperature of the temperature T of mould a little more than high molecular polymer simultaneously;
5) set the pulling speed of extrusion speed and the towing mechanism of pushing mechanism, and make pulling speed identical with extrusion speed, then start squeezing device, the process furnace group is heated container, makes chalcogenide glass and high molecular polymer in container be subject to thermal softening; Pushing mechanism by the chalcogenide glass after softening and high molecular polymer slowly, extrude equably; The rod that extrudes of extruding is brought down a fever and is pulled device through the stove of bringing down a fever and draws;
6) rod that extrudes that will draw is annealed after 4 ~ 6h under the transition temperature Tg of chalcogenide glass, then slow cooling is to room temperature; Obtain the chalcogenide glass fiber prefabricated rods.
Preferably, described high molecular polymer is any one in polyphenylene sulfide, polyimide, polysulfones, polyethersulfone and polyarylsulphone; Described rare gas element is nitrogen or argon gas.
Compared with prior art, the invention has the advantages that: superposition method of the present invention extrudes the squeezing device of chalcogenide glass fiber prefabricated rods, its container is outside equipped with the process furnace group, the bottom of container is provided with the stove of bringing down a fever, the bring down a fever bottom of stove is provided with towing mechanism, set during use and make pulling speed identical with extrusion speed, in the time of can guaranteeing that like this chalcogenide glass fiber prefabricated rods is extruded, the homogeneity that its structure forms is not subject to the impact of gravity; Squeezing device and method that superposition method of the present invention extrudes the chalcogenide glass fiber prefabricated rods have the advantages that controllability is good, production efficiency is high; Adopt superposition method extruding chalcogenide glass; the structure of the chalcogenide glass fiber prefabricated rods obtained forms evenly, surfaces externally and internally is smooth, interface is desirable; and the top layer of the chalcogenide glass fiber prefabricated rods obtained has the protective layer be comprised of high molecular polymer, be convenient to the performance test after pulling optical fiber preform.
The accompanying drawing explanation
The structural representation that Fig. 1 is the embodiment squeezing device.
Embodiment
Below in conjunction with accompanying drawing, embodiment is described in further detail the present invention.
As shown in Figure 1, a kind of superposition method extrudes the squeezing device of chalcogenide glass fiber prefabricated rods, comprise pushing mechanism 1, extrusion stem 2, container 3, pressure pad 4, mould 5, temperature controls platform 6 and computer is controlled platform 7, pushing mechanism 1 is arranged on the top of container 3, extrusion stem 2 is fixedly connected with pushing mechanism 1, pressure pad 4 is fixedly connected with extrusion stem 2, container 3 is outside equipped with the process furnace group for container 3 is heated, the process furnace group comprises the first process furnace 81 and the second process furnace 82, the first process furnace 81 is arranged on the top of container 3, the second process furnace 82 is arranged on the bottom of container 3, the process furnace group is outside equipped with vacuum chamber 9, vacuum chamber 9 is connected with vacuum pump 91, pressure pad 4 is arranged in container 3, the lower end of container 3 is provided with extrusion 32, mould 5 is arranged on the bottom of container 3, the nib 51 of mould 5 is connected with extrusion 32, the bottom of container 3 is provided with the stove 10 of bringing down a fever of being annealed for the preform to extruding, the bring down a fever bottom of stove 10 is provided with towing mechanism 11, bring down a fever between stove 10 and towing mechanism 11 and be provided with for preventing from extruding the locating device 12 that rod is crooked.
The arranged outside of container 3 has temperature sensor 31, and temperature sensor 31, the first process furnace 81, the second process furnace 82 and the stove 10 of bringing down a fever are all controlled platform 6 with temperature and be connected.
Pushing mechanism 1 is provided with pressure warning unit 14, and pressure warning unit is connected with pressure-display device 13.
Computer is controlled platform 7 and is connected with temperature sensor 31 with pressure transmitter 21 respectively.
In above squeezing device, the surface of the internal surface of container 3 and mould 5 can be coated with graphite linings.
Utilize above-mentioned squeezing device to extrude the chalcogenide glass of different components, prepare preform:
Embodiment mono-: the chalcogenide glass that the component of take is sulfide, selenide and stibnide extrudes preform, the T of this chalcogenide glass>100 ℃, and T=Tx-Tg wherein, Tx should be recrystallization temperature of chalcogenide glass, the transition temperature that Tg is this chalcogenide glass; Its extruding method comprises the following steps: 1) be ready to chalcogenide glass and the polyethersulfone (PES) of polylith sheet, with alcohol, rinse post-drying, put into vacuum vessel; 2) at first take out a slice polyethersulfone, then the chalcogenide glass of the polylith sheet that superposes successively on the top of this sheet polyethersulfone, then the polyethersulfone after stack is put into to container together with chalcogenide glass, and make high molecular polymer be placed on the lowermost end of container; 3) utilize vacuum pump to vacuumize vacuum chamber, when the low vacuum of vacuum chamber in 10
-2during Pa, to topping up in vacuum chamber, this rare gas element can be nitrogen or argon gas, makes the air pressure in vacuum chamber identical with external atmosphere pressure; 4) open temperature and control platform, set the process furnace group and the temperature of the stove of bringing down a fever, and the temperature T of setting mould is Tg<T<Tx, make the softening temperature of the temperature T of mould a little more than high molecular polymer simultaneously; 5) set the pulling speed of extrusion speed and the towing mechanism of pushing mechanism, and make pulling speed identical with extrusion speed, the homogeneity that structure when guaranteeing that chalcogenide glass is extruded forms is not subject to the impact of gravity, then start squeezing device, the process furnace group is heated container, makes chalcogenide glass and polyethersulfone in container be subject to thermal softening; Pushing mechanism by the chalcogenide glass after softening and polyethersulfone slowly, extrude equably; The rod that extrudes of extruding is brought down a fever and is pulled device through the stove of bringing down a fever and draws; The labview programming software that computer is controlled in platform reads and records squeeze and the time dependent data of extrusion temperature; That 6) will draw extrudes rod under the transition temperature Tg of chalcogenide glass after annealing 4h, then slow cooling is to room temperature; Obtain the preform of embodiment mono-.
Embodiment bis-: the chalcogenide glass that the component of take is sulfide and selenide extrudes preform, the T of this chalcogenide glass>240 ℃, T=Tx-Tg wherein, the recrystallization temperature that Tx is this chalcogenide glass, the transition temperature that Tg is this chalcogenide glass; Its extruding method comprises the following steps: 1) be ready to chalcogenide glass and the polysulfones (PSU) of polylith sheet, with alcohol, rinse post-drying, put into vacuum vessel; 2) at first take out a slice polysulfones, then the chalcogenide glass of the polylith sheet that superposes successively on the top of this sheet polysulfones, then the polysulfones after stack is put into to container together with chalcogenide glass, and make high molecular polymer be placed on the lowermost end of container; 3) utilize vacuum pump to vacuumize vacuum chamber, when the low vacuum of vacuum chamber in 10
-2during Pa, to topping up in vacuum chamber, this rare gas element can be nitrogen or argon gas, makes the air pressure in vacuum chamber identical with external atmosphere pressure; 4) open temperature and control platform, set the process furnace group and the temperature of the stove of bringing down a fever, and the temperature T of setting mould is Tg<T<Tx, make the softening temperature of the temperature T of mould a little more than high molecular polymer simultaneously; 5) set the pulling speed of extrusion speed and the towing mechanism of pushing mechanism, and make pulling speed identical with extrusion speed, the homogeneity that structure when guaranteeing that chalcogenide glass is extruded forms is not subject to the impact of gravity, then start squeezing device, the process furnace group is heated container, makes chalcogenide glass and polysulfones in container be subject to thermal softening; Pushing mechanism by the chalcogenide glass after softening and polysulfones slowly, extrude equably; The rod that extrudes of extruding is brought down a fever and is pulled device through the stove of bringing down a fever and draws; The labview programming software that computer is controlled in platform reads and records squeeze and the time dependent data of extrusion temperature; That 6) will draw extrudes rod under the transition temperature Tg of chalcogenide glass after annealing 5h, then slow cooling is to room temperature; Obtain the preform of embodiment bis-.
Embodiment tri-: the chalcogenide glass that the component of take is sulfide, selenide and telluride extrudes preform, the T of this chalcogenide glass>150 ℃, T=Tx-Tg wherein, the recrystallization temperature that Tx is this chalcogenide glass, the transition temperature that Tg is this chalcogenide glass; Its extruding method comprises the following steps: 1) be ready to chalcogenide glass and the polyimide (PI) of polylith sheet, with alcohol, rinse post-drying, put into vacuum vessel; 2) at first take out a slice polyimide, the chalcogenide glass of the polylith sheet that superposes successively on the top of this sheet polyimide again, then the polyimide after stack is put into to container together with chalcogenide glass, and make high molecular polymer be placed on the lowermost end of container; 3) utilize vacuum pump to vacuumize vacuum chamber, when the low vacuum of vacuum chamber in 10
-2during Pa, to topping up in vacuum chamber, this rare gas element can be nitrogen or argon gas, makes the air pressure in vacuum chamber identical with external atmosphere pressure; 4) open temperature and control platform, set the process furnace group and the temperature of the stove of bringing down a fever, and the temperature T of setting mould is Tg<T<Tx, make the softening temperature of the temperature T of mould a little more than high molecular polymer simultaneously; 5) set the pulling speed of extrusion speed and the towing mechanism of pushing mechanism, and make pulling speed identical with extrusion speed, the homogeneity that structure when guaranteeing that chalcogenide glass is extruded forms is not subject to the impact of gravity, then start squeezing device, the process furnace group is heated container, makes chalcogenide glass and polyimide in container be subject to thermal softening; Pushing mechanism by the chalcogenide glass after softening and polyimide slowly, extrude equably; The rod that extrudes of extruding is brought down a fever and is pulled device through the stove of bringing down a fever and draws; The labview programming software that computer is controlled in platform reads and records squeeze and the time dependent data of extrusion temperature; That 6) will draw extrudes rod under the transition temperature Tg of chalcogenide glass after annealing 6h, then slow cooling is to room temperature; Obtain the preform of embodiment tri-.
Embodiment tetra-: the chalcogenide glass that the component of take is telluride and sulfide extrudes preform, the T of this chalcogenide glass>220 ℃, T=Tx-Tg wherein, the recrystallization temperature that Tx is this chalcogenide glass, the transition temperature that Tg is this chalcogenide glass; Its extruding method comprises the following steps: 1) be ready to the chalcogenide glass of polylith sheet and the polyphenylene sulfide (PPS) that softening temperature is 260 ~ 320 ℃, with alcohol, rinse post-drying, put into vacuum vessel; 2) at first take out a slice polyphenylene sulfide, the chalcogenide glass of the polylith sheet that superposes successively on the top of this sheet polyphenylene sulfide again, then the polyphenylene sulfide after stack is put into to container together with chalcogenide glass, and make high molecular polymer be placed on the lowermost end of container; 3) utilize vacuum pump to vacuumize vacuum chamber, when the low vacuum of vacuum chamber in 10
-2during Pa, to topping up in vacuum chamber, this rare gas element can be nitrogen or argon gas, makes the air pressure in vacuum chamber identical with external atmosphere pressure; 4) open temperature and control platform, set the process furnace group and the temperature of the stove of bringing down a fever, and the temperature T of setting mould is Tg<T<Tx, make the softening temperature of the temperature T of mould a little more than high molecular polymer simultaneously; 5) set the pulling speed of extrusion speed and the towing mechanism of pushing mechanism, and make pulling speed identical with extrusion speed, the homogeneity that structure when guaranteeing that chalcogenide glass is extruded forms is not subject to the impact of gravity, then start squeezing device, the process furnace group is heated container, makes chalcogenide glass and polyphenylene sulfide in container be subject to thermal softening; Pushing mechanism by the chalcogenide glass after softening and polyphenylene sulfide slowly, extrude equably; The rod that extrudes of extruding is brought down a fever and is pulled device through the stove of bringing down a fever and draws; The labview programming software that computer is controlled in platform reads and records squeeze and the time dependent data of extrusion temperature; That 6) will draw extrudes rod under the transition temperature Tg of chalcogenide glass after annealing 6h, then slow cooling is to room temperature; Obtain the preform of embodiment tetra-.
The chalcogenide glass fiber prefabricated rods of above-described embodiment one ~ embodiment tetra-obtained, its structure forms evenly, surfaces externally and internally is smooth, interface is desirable, and top layer has the protective layer be comprised of high molecular polymer, is convenient to the performance test after drawing optical fiber.
Claims (10)
1. superposition method extrudes the squeezing device of chalcogenide glass fiber prefabricated rods, comprise pushing mechanism, extrusion stem, container, pressure pad and mould, it is characterized in that described pushing mechanism is arranged on the top of described container, described extrusion stem is fixedly connected with described pushing mechanism, described container is outside equipped with the process furnace group for described container is heated, described process furnace group is outside equipped with vacuum chamber, described vacuum chamber is connected with vacuum pump, described pressure pad is arranged in described container, the lower end of described container is provided with extrusion, described mould is arranged on the bottom of described container, the nib of described mould is connected with described extrusion, the bottom of described container is provided with the stove of bringing down a fever of being annealed for the preform to extruding, the bottom of the described stove of bringing down a fever is provided with towing mechanism.
2. superposition method according to claim 1 extrudes the squeezing device of chalcogenide glass fiber prefabricated rods, it is characterized in that described pressure pad is fixedly connected with described extrusion stem; Described bringing down a fever between stove and described towing mechanism is provided with for preventing from extruding the locating device that rod is crooked.
3. superposition method according to claim 1 and 2 extrudes the squeezing device of chalcogenide glass fiber prefabricated rods, it is characterized in that described process furnace group comprises the first process furnace and the second process furnace, described the first process furnace is arranged on the top of described container, and described the second process furnace is arranged on the bottom of described container.
4. superposition method according to claim 3 extrudes the squeezing device of chalcogenide glass fiber prefabricated rods, characterized by further comprising temperature and control platform, the arranged outside of described container has temperature sensor, and described temperature sensor, described the first process furnace, described the second process furnace are all controlled platform with described temperature with the described stove of bringing down a fever and be connected.
5. superposition method according to claim 4 extrudes the squeezing device of chalcogenide glass fiber prefabricated rods, it is characterized in that, on described extrusion stem, pressure transmitter is installed, one end of described pressure transmitter is connected with a pressure-display device, and the other end of described pressure transmitter is connected with described pushing mechanism.
6. superposition method according to claim 5 extrudes the squeezing device of chalcogenide glass fiber prefabricated rods, it is characterized in that described pushing mechanism is provided with pressure warning unit, and described pressure warning unit is connected with described pressure-display device.
7. superposition method according to claim 6 extrudes the squeezing device of chalcogenide glass fiber prefabricated rods, characterized by further comprising computer and controls platform, and described computer is controlled platform and is connected with described temperature sensor with described pressure transmitter respectively.
8. superposition method according to claim 1 and 2 extrudes the squeezing device of chalcogenide glass fiber prefabricated rods, it is characterized in that the internal surface of described container and the surface-coated of described mould have graphite linings.
9. superposition method extrudes the method for chalcogenide glass fiber prefabricated rods, it is characterized in that comprising the following steps:
1) be ready to chalcogenide glass and the high molecular polymer of polylith sheet, with alcohol, rinse post-drying, put into vacuum vessel;
2) at first take out a slice high molecular polymer, the chalcogenide glass of the polylith sheet that superposes successively on the top of this sheet high molecular polymer again, then the high molecular polymer after stack is put into to container together with chalcogenide glass, and make high molecular polymer be placed on the lowermost end of container;
3) utilize vacuum pump to vacuumize vacuum chamber, when the low vacuum of vacuum chamber in 10
-2during Pa, to topping up in vacuum chamber, make the air pressure in vacuum chamber identical with external atmosphere pressure;
4) open temperature and control platform, set the process furnace group and the temperature of stove of bringing down a fever, and the temperature T of setting mould is Tg<T<Tx, the recrystallization temperature that wherein Tx is chalcogenide glass, the transition temperature that Tg is chalcogenide glass makes the softening temperature of the temperature T of mould a little more than high molecular polymer simultaneously;
5) set the pulling speed of extrusion speed and the towing mechanism of pushing mechanism, and make pulling speed identical with extrusion speed, then start squeezing device, the process furnace group is heated container, makes chalcogenide glass and high molecular polymer in container be subject to thermal softening; Pushing mechanism by the chalcogenide glass after softening and high molecular polymer slowly, extrude equably; The rod that extrudes of extruding is brought down a fever and is pulled device through the stove of bringing down a fever and draws;
6) rod that extrudes that will draw is annealed after 4 ~ 6h under the transition temperature Tg of chalcogenide glass, then slow cooling is to room temperature; Obtain the chalcogenide glass fiber prefabricated rods.
10. superposition method according to claim 9 extrudes the method for chalcogenide glass fiber prefabricated rods, it is characterized in that the T of described chalcogenide glass>100 ℃, wherein T=Tx-Tg; Described high molecular polymer is any one in polyphenylene sulfide, polyimide, polysulfones, polyethersulfone and polyarylsulphone; Described rare gas element is nitrogen or argon gas.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310364102.7A CN103466933B (en) | 2013-08-20 | 2013-08-20 | Superposition method extrudes squeezing device and the method for chalcogenide glass fiber prefabricated rods |
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| CN104529151A (en) * | 2015-01-22 | 2015-04-22 | 宁波大学 | Preparation method and preparation equipment of optical fiber preform |
| CN104817263A (en) * | 2015-04-18 | 2015-08-05 | 江苏师范大学 | Double-sleeve extrusion die for extruding chalcogenide glass optical fiber preform rod and use method |
| CN105271696A (en) * | 2015-10-12 | 2016-01-27 | 宁波大学 | Fiber core-cladding ratio adjustable optical fiber preform extrusion method and device |
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| CN104529151A (en) * | 2015-01-22 | 2015-04-22 | 宁波大学 | Preparation method and preparation equipment of optical fiber preform |
| CN104529151B (en) * | 2015-01-22 | 2017-01-04 | 宁波大学 | The preparation method of a kind of preform and Preparation equipment |
| CN104817263A (en) * | 2015-04-18 | 2015-08-05 | 江苏师范大学 | Double-sleeve extrusion die for extruding chalcogenide glass optical fiber preform rod and use method |
| CN104817263B (en) * | 2015-04-18 | 2017-05-03 | 江苏师范大学 | Double-sleeve extrusion die for extruding chalcogenide glass optical fiber preform rod and use method |
| CN105271696A (en) * | 2015-10-12 | 2016-01-27 | 宁波大学 | Fiber core-cladding ratio adjustable optical fiber preform extrusion method and device |
| CN105271696B (en) * | 2015-10-12 | 2018-02-16 | 宁波大学 | The adjustable preform extruding method of fibre core covering ratio and device |
| CN105642691A (en) * | 2016-03-22 | 2016-06-08 | 中国重型机械研究院股份公司 | Aluminum base ceramic powder reinforced composite material extruding device and extruding method |
| CN105923988A (en) * | 2016-05-12 | 2016-09-07 | 宁波大学 | Extruding preparation method of elliptical core polarization maintaining optical fiber perform rod with ellipticity adjustable at random |
| CN106045284B (en) * | 2016-06-01 | 2019-02-19 | 中国建筑材料科学研究总院 | A kind of manufacturing process of chalcogenide glass |
| CN106045284A (en) * | 2016-06-01 | 2016-10-26 | 中国建筑材料科学研究总院 | Forming method of chalcogenide glass |
| CN106122776A (en) * | 2016-06-30 | 2016-11-16 | 东莞轩朗实业有限公司 | The production method of quantum dot Rhizoma Dioscoreae (peeled) |
| CN106122776B (en) * | 2016-06-30 | 2019-01-25 | 东莞轩朗实业有限公司 | The production method of quantum dot striation |
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| CN106966571B (en) * | 2017-05-08 | 2023-02-03 | 宁波舜宇红外技术有限公司 | Preparation method and preparation device of glass rod material |
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| CN107311444A (en) * | 2017-07-11 | 2017-11-03 | 中国科学院上海光学精密机械研究所 | The pressurizing unit and preparation method of preform |
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| CN107601901A (en) * | 2017-09-19 | 2018-01-19 | 武汉理工大学 | A kind of glass ceramics and preparation method thereof and the application as material of infrared window |
| CN108751694A (en) * | 2018-04-16 | 2018-11-06 | 江苏师范大学 | A kind of preparation method of the infrared chalcogenide glass fiber coherent fiber bundle of high fill-factor |
| CN108751694B (en) * | 2018-04-16 | 2021-05-28 | 江苏师范大学 | Preparation method of infrared chalcogenide glass optical fiber image transmission bundle with high filling coefficient |
| CN108516668A (en) * | 2018-04-28 | 2018-09-11 | 中国建筑材料科学研究总院有限公司 | A kind of secondary drawing device of glass tube and method |
| CN108516668B (en) * | 2018-04-28 | 2021-03-16 | 中国建筑材料科学研究总院有限公司 | Secondary drawing device and method for glass tube |
| CN110357403B (en) * | 2019-08-08 | 2021-10-19 | 中国建筑材料科学研究总院有限公司 | Chalcogenide glass rod forming device and method |
| CN110357403A (en) * | 2019-08-08 | 2019-10-22 | 中国建筑材料科学研究总院有限公司 | Chalcogenide glass bar molding machine and method |
| CN112358177A (en) * | 2020-11-11 | 2021-02-12 | 安徽省绩溪县华宇防火滤料有限公司 | Processing device for glass fibers |
| CN112499942A (en) * | 2020-12-24 | 2021-03-16 | 安徽光智科技有限公司 | Extrusion process method of chalcogenide glass |
| CN113233745A (en) * | 2021-05-18 | 2021-08-10 | 杭州长波红外科技有限公司 | Atmosphere protection type chalcogenide glass rod extrusion equipment and operation process thereof |
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