CN103466933B - Superposition method extrudes squeezing device and the method for chalcogenide glass fiber prefabricated rods - Google Patents
Superposition method extrudes squeezing device and the method for chalcogenide glass fiber prefabricated rods Download PDFInfo
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- CN103466933B CN103466933B CN201310364102.7A CN201310364102A CN103466933B CN 103466933 B CN103466933 B CN 103466933B CN 201310364102 A CN201310364102 A CN 201310364102A CN 103466933 B CN103466933 B CN 103466933B
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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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- 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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Abstract
The invention discloses squeezing device and method that superposition method extrudes chalcogenide glass fiber prefabricated rods, the pushing mechanism of this squeezing device is arranged on the top of container, extrusion stem is fixedly connected with pushing mechanism, container is outside equipped with the process furnace group for heating container, process furnace group is outside equipped with vacuum chamber, vacuum chamber is connected with vacuum pump, pressure pad is arranged in container, the lower end of container is provided with extrusion, mould is arranged on the bottom of container, the nib of mould is connected with extrusion, the bottom of container is provided with the stove of bringing down a fever for annealing to the preform extruded, the bring down a fever bottom of stove is provided with towing mechanism.Squeezing device of the present invention and method have the advantages that controllability is good, production efficiency is high; Adopt superposition method extruding chalcogenide glass, the structure composition of the preform obtained evenly, surfaces externally and internally is smooth, interface is desirable, and top layer has the protective layer be made up of high molecular polymer, is convenient to the performance test after drawing optical fiber.
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 chalcogenide glass fiber prefabricated rods.
Background technology
In telecommunication optical fiber preparation process, one of important content is the preparation of preform, preform technology of preparing traditional at present has four kinds of techniques, and these four kinds of techniques are respectively Outside Vapor Deposition (OVD), vapour phase axial deposition technique (VAD), improve vapour deposition process (MCVD) and plasma activated chemical vapour deposition technique (PCVD).Recent two decades comes, OVD method develops into many blowtorch from single spraying lamp deposition and deposits simultaneously, sedimentation rate is multiplied, realize an equipment and deposit many rods simultaneously, and develop into two step method from the single stage method depositing core covering successively and make prefabricated rods, namely first prepare large diameter plug, be drawn into minor diameter plug or not drawing-down again, then adopt surrounding layer technology to prepare preform, improve production efficiency, reduce production cost.But MCVD method, especially PCVD method, OVD method and VAD method more easily accurately control the radial refractive index distribution of plug, thus for preparing multimode optical fibers MMF and non-zero dispersion fiber DZDF core prefabricated rods is more effective.
Chalcogenide glass has excellent mid and far infrared through performance, and specific refractory power is high, and has high nonlinear viscoelastic piles etc.Due to the infrared transmission performance that it is excellent, 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, is 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 inventions such as the Monro of Southampton University of Southampton.2006, French Perfos company and French reyn 1 university combined the baroque Ga of one reporting and adopt method of piling to prepare
5ge
20sb
10se
65microstructured optical fibers.Although method of piling is the making method of chalcogenide glass fiber prefabricated rods the most ripe at present, but method of piling workload is large, easily there is defect in easily crisp chalcogenide glass tubule surface, and add in hot-stretching step form kapillary boundling arrangement kapillary inside easily occur that airport subsides and is out of shape, the defect such as crystallization particle, bubble between kapillary interface is also more, merges inadequate generated interfacial air defect based on gap between kapillary in collapse process.Because adopt air pressure hierarchical control to be difficult to making and the wire drawing of the many pores prefabricated rods accurately controlling complex construction, so cause the chalcogenide glass microstructured optical fibers loss of preparation general higher.
Casting is the preparation method of the another kind of chalcogenide glass fiber prefabricated rods that 2010 are invented by the people such as Quentin Coulombier of French reyn 1 university.Its process is roughly: flowed into by the chalcogenide glass of the molten state after purifying in the quartzy frame body constructed with quartzy solid slim rods by how in the silica tube that vacuum high-temperature is closed, the quartzy thin slice of perforation is fixed on before and after thin rod, bond after two quartzy thin slice oxyhydrogen flame heating with quartzy tube wall in advance, after high temperature is fully founded, silica tube is holded up, glass metal is made to flow in the frame body of solid bar composition, fine annealing after quenching, the chalcogenide glass prepared rod is inserted the hydrofluoric acid dips that concentration is 40%, thin for quartz rod is dissolved, thus obtain chalcogenide glass fiber prefabricated rods.Compared with method of piling, casting has clear superiority: such as casting technique is simple, avoids the arrangement out of true that method of piling accumulation capillary glass tube arrangement human factor causes, easily prepares the preform etc. of different cross section structure.But, for the chalcogenide glass fiber prefabricated rods that casting prepares, the chalcogenide glass microstructured optical fibers of follow-up preparation also has certain defect, can not prepare the microstructured optical fibers that core covering component is different, and the smooth finish of the hole inwall corroded after inner quartz rod is still a key issue.
Although method of piling and casting have the case successfully producing chalcogenide glass fiber prefabricated rods, the fibre loss of producing due to these two kinds of methods is all very large, and technics comparing is complicated, is not suitable for large-scale production.Therefore be necessary the preparation method developing the chalcogenide glass fiber prefabricated rods made new advances, improve quality and the production efficiency of chalcogenide glass fiber prefabricated rods.At present domestic prepared by the patent of sulphur system preform for superposition method and document less, wherein domestic patent CN1081654A is kind of the method manufacturing preform, mainly can obtain one there is higher mechanical strength and do not have alveolate plastic optical fiber, instead of relate to the preparation of chalcogenide glass fiber prefabricated rods.What patent CN102531377 introduced is a kind of vacuum extruder for the preparation of chalcogenide glass fiber prefabricated rods, by the extruding of extrusion machine to chalcogenide glass, make the glass softened through mould, chalcogenide glass more annealed process can obtain chalcogenide glass fiber prefabricated rods, when but chalcogenide glass fiber prefabricated rods is prepared in the extruding of this extrusion machine, its prefabricated rods extruded is larger by the impact of gravity, the structure of prefabricated rods is caused to form the various defects such as uneven, production efficiency is not high, and has a negative impact to the quality of the optical fiber of follow-up drawing.
Summary of the invention
Technical problem to be solved by this invention is: for the deficiencies in the prior art, provides 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 heating described container, 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 for annealing to the preform extruded, the bottom of described stove of bringing down a fever is provided with towing mechanism.
Preferably, described pressure pad is fixedly connected with described extrusion stem; Described bring down a fever to be provided with between stove and described towing mechanism extrude the bending locating device of rod for preventing.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 the first described process furnace is arranged on the top of described container, and the second described process furnace is arranged on the bottom of described container.During use according to the component of chalcogenide glass and high molecular polymer and compression properties different, set the first different process furnace and the temperature of 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, the first described process furnace, the second described process furnace are all connected with described temperature control platform with described stove of bringing down a fever.Temperature control platform accurately can control the temperature of the first process furnace, the second process furnace and stove of bringing down a fever, and ensure that accuracy and the controllability of temperature in extruding and process of bringing down a fever.Simultaneous temperature parametric controller can be monitored actual extrusion temperature during extruding, and when actual extrusion temperature exceedes the extrusion temperature of setting, temperature control platform can automatic alarm.
Preferably, described extrusion stem is provided with pressure transmitter, 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.Pressure transmitter and pressure-display device, can provide 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 is higher than the squeeze set, pressure warning unit is reported to the police, and pushing mechanism quits work automatically.
Preferably, also comprise conputer controlled platform, described conputer controlled platform is connected with described temperature sensor with described pressure transmitter respectively.Conputer controlled platform can record squeeze and the time dependent data of extrusion temperature, enhances the controllability of extrusion process.
Preferably, the internal surface of described container and the surface-coated of described mould have graphite linings.Graphite has excellent thermotolerance, and in addition, after container and mould apply graphite linings, the surface of the preform extruded also can be attached with graphite, has certain provide protection to the preform extruded.
Superposition method extrudes the method for chalcogenide glass fiber prefabricated rods, comprises the following steps:
1) get out chalcogenide glass and the high molecular polymer of polylith sheet, use alcohol rinse post-drying, put into vacuum vessel;
2) first a slice high molecular polymer is taken out, the chalcogenide glass of polylith sheet is superposed again successively on the top of this sheet high molecular polymer, then the high molecular polymer after superposition is put into container together with chalcogenide glass, and make high molecular polymer be placed on the lowermost end of container;
3) vacuum pump is utilized to vacuumize vacuum chamber, when the low vacuum of vacuum chamber is in 10
-2during Pa, topping up in vacuum chamber, makes the air pressure in vacuum chamber identical with external atmosphere pressure;
4) temperature control platform is opened, set process furnace group and the temperature of stove of bringing down a fever, and the temperature T setting mould is Tg<T<Tx, wherein Tx is the recrystallization temperature of chalcogenide glass, Tg is the transition temperature of chalcogenide glass, makes the softening temperature of temperature T a little more than high molecular polymer of mould simultaneously;
5) extrusion speed of pushing mechanism and the pulling speed of towing mechanism is set, and make pulling speed identical with extrusion speed, then start squeezing device, process furnace group heats container, makes the chalcogenide glass in container and high molecular polymer be subject to thermal softening; Chalcogenide glass after softening and high molecular polymer slowly, are equably extruded by pushing mechanism; The rod that extrudes extruded is brought down a fever through stove of bringing down a fever and is pulled device extraction;
6) extrude rod under the transition temperature Tg of chalcogenide glass after annealing 4 ~ 6h by what draw, then slow cooling is to room temperature; Namely chalcogenide glass fiber prefabricated rods is obtained.
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 process furnace group, the bottom of container is provided with 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, when can ensure that chalcogenide glass fiber prefabricated rods is extruded like this, the homogeneity of its structure composition is not by the impact of gravity; Superposition method of the present invention extrudes the squeezing device of chalcogenide glass fiber prefabricated rods and method has the advantages that controllability is good, production efficiency is high; Adopt superposition method extruding chalcogenide glass; the structure composition of the chalcogenide glass fiber prefabricated rods obtained 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 made up of high molecular polymer, is convenient to the performance test after pulling optical fiber preform.
Accompanying drawing explanation
Fig. 1 is the structural representation of embodiment squeezing device.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
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 control platform 6 and conputer 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 heating container 3, process furnace group comprises the first process furnace 81 and the second process furnace 82, first process furnace 81 is arranged on the top of container 3, second process furnace 82 is arranged on the bottom of container 3, 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 for annealing to the preform extruded, the bring down a fever bottom of stove 10 is provided with towing mechanism 11, bring down a fever to be provided with between stove 10 and towing mechanism 11 and extrude the bending locating device 12 of rod for preventing.
The arranged outside of container 3 has temperature sensor 31, and temperature sensor 31, first process furnace 81, second process furnace 82 is all connected with temperature control platform 6 with stove 10 of bringing down a fever.
Extrusion stem 2 is provided with pressure transmitter 21, one end of pressure transmitter 21 is connected with a pressure-display device 13, and the other end of pressure transmitter 21 is connected with pushing mechanism 1.
Pushing mechanism 1 is provided with pressure warning unit 14, and pressure warning unit is connected with pressure-display device 13.
Conputer controlled platform 7 is connected with temperature sensor 31 with pressure transmitter 21 respectively.
In above squeezing device, the internal surface of container 3 and the surface of mould 5 can be coated with graphite linings.
Utilize above-mentioned squeezing device to extrude the chalcogenide glass of different components, prepare preform:
Embodiment one: be that the chalcogenide glass of sulfide, selenide and stibnide extrudes preform with component, the T > of this chalcogenide glass 100 DEG C, wherein T=Tx-Tg, Tx should be the recrystallization temperature of chalcogenide glass, and Tg is the transition temperature of this chalcogenide glass; Its extruding method comprises the following steps: the chalcogenide glass and the polyethersulfone (PES) that 1) get out polylith sheet, uses alcohol rinse post-drying, puts into vacuum vessel; 2) first take out a slice polyethersulfone, then superpose the chalcogenide glass of polylith sheet on the top of this sheet polyethersulfone successively, then the polyethersulfone after superposition is put into container together with chalcogenide glass, and make high molecular polymer be placed on the lowermost end of container; 3) vacuum pump is utilized to vacuumize vacuum chamber, when the low vacuum of vacuum chamber is in 10
-2during Pa, 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 control platform, set process furnace group and the temperature of stove of bringing down a fever, and the temperature T setting mould is Tg<T<Tx, makes the softening temperature of temperature T a little more than high molecular polymer of mould simultaneously; 5) extrusion speed of pushing mechanism and the pulling speed of towing mechanism is set, and make pulling speed identical with extrusion speed, the homogeneity of structure composition during to ensure that chalcogenide glass is extruded is by the impact of gravity, then squeezing device is started, process furnace group heats container, makes the chalcogenide glass in container and polyethersulfone be subject to thermal softening; Chalcogenide glass after softening and polyethersulfone slowly, are equably extruded by pushing mechanism; The rod that extrudes extruded is brought down a fever through stove of bringing down a fever and is pulled device extraction; Labview programming software in conputer controlled platform reads and records squeeze and the time dependent data of extrusion temperature; 6) rod that extrudes of drawing is annealed after 4h under the transition temperature Tg of chalcogenide glass, then slow cooling is to room temperature; Namely the preform of embodiment one is obtained.
Embodiment two: be that the chalcogenide glass of sulfide and selenide extrudes preform, the T > of this chalcogenide glass 240 DEG C with component, wherein T=Tx-Tg, Tx are the recrystallization temperature of this chalcogenide glass, and Tg is the transition temperature of this chalcogenide glass; Its extruding method comprises the following steps: the chalcogenide glass and the polysulfones (PSU) that 1) get out polylith sheet, uses alcohol rinse post-drying, puts into vacuum vessel; 2) first take out a slice polysulfones, then superpose the chalcogenide glass of polylith sheet on the top of this sheet polysulfones successively, then the polysulfones after superposition is put into container together with chalcogenide glass, and make high molecular polymer be placed on the lowermost end of container; 3) vacuum pump is utilized to vacuumize vacuum chamber, when the low vacuum of vacuum chamber is in 10
-2during Pa, 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 control platform, set process furnace group and the temperature of stove of bringing down a fever, and the temperature T setting mould is Tg<T<Tx, makes the softening temperature of temperature T a little more than high molecular polymer of mould simultaneously; 5) extrusion speed of pushing mechanism and the pulling speed of towing mechanism is set, and make pulling speed identical with extrusion speed, the homogeneity of structure composition during to ensure that chalcogenide glass is extruded is by the impact of gravity, then squeezing device is started, process furnace group heats container, makes the chalcogenide glass in container and polysulfones be subject to thermal softening; Chalcogenide glass after softening and polysulfones slowly, are equably extruded by pushing mechanism; The rod that extrudes extruded is brought down a fever through stove of bringing down a fever and is pulled device extraction; Labview programming software in conputer controlled platform reads and records squeeze and the time dependent data of extrusion temperature; 6) rod that extrudes of drawing is annealed after 5h under the transition temperature Tg of chalcogenide glass, then slow cooling is to room temperature; Namely the preform of embodiment two is obtained.
Embodiment three: be that the chalcogenide glass of sulfide, selenide and telluride extrudes preform with component, the T > of this chalcogenide glass 150 DEG C, wherein T=Tx-Tg, Tx are the recrystallization temperature of this chalcogenide glass, and Tg is the transition temperature of this chalcogenide glass; Its extruding method comprises the following steps: the chalcogenide glass and the polyimide (PI) that 1) get out polylith sheet, uses alcohol rinse post-drying, puts into vacuum vessel; 2) first a slice polyimide is taken out, the chalcogenide glass of polylith sheet is superposed again successively on the top of this sheet polyimide, then the polyimide after superposition is put into container together with chalcogenide glass, and make high molecular polymer be placed on the lowermost end of container; 3) vacuum pump is utilized to vacuumize vacuum chamber, when the low vacuum of vacuum chamber is in 10
-2during Pa, 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 control platform, set process furnace group and the temperature of stove of bringing down a fever, and the temperature T setting mould is Tg<T<Tx, makes the softening temperature of temperature T a little more than high molecular polymer of mould simultaneously; 5) extrusion speed of pushing mechanism and the pulling speed of towing mechanism is set, and make pulling speed identical with extrusion speed, the homogeneity of structure composition during to ensure that chalcogenide glass is extruded is by the impact of gravity, then squeezing device is started, process furnace group heats container, makes the chalcogenide glass in container and polyimide be subject to thermal softening; Chalcogenide glass after softening and polyimide slowly, are equably extruded by pushing mechanism; The rod that extrudes extruded is brought down a fever through stove of bringing down a fever and is pulled device extraction; Labview programming software in conputer controlled platform reads and records squeeze and the time dependent data of extrusion temperature; 6) rod that extrudes of drawing is annealed after 6h under the transition temperature Tg of chalcogenide glass, then slow cooling is to room temperature; Namely the preform of embodiment three is obtained.
Embodiment four: be that the chalcogenide glass of telluride and sulfide extrudes preform, the T > of this chalcogenide glass 220 DEG C with component, wherein T=Tx-Tg, Tx are the recrystallization temperature of this chalcogenide glass, and Tg is the transition temperature of this chalcogenide glass; Its extruding method comprises the following steps: 1) get out the polyphenylene sulfide (PPS) that the chalcogenide glass of polylith sheet and softening temperature are 260 ~ 320 DEG C, use alcohol rinse post-drying, put into vacuum vessel; 2) first a slice polyphenylene sulfide is taken out, the chalcogenide glass of polylith sheet is superposed again successively on the top of this sheet polyphenylene sulfide, then the polyphenylene sulfide after superposition is put into container together with chalcogenide glass, and make high molecular polymer be placed on the lowermost end of container; 3) vacuum pump is utilized to vacuumize vacuum chamber, when the low vacuum of vacuum chamber is in 10
-2during Pa, 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 control platform, set process furnace group and the temperature of stove of bringing down a fever, and the temperature T setting mould is Tg<T<Tx, makes the softening temperature of temperature T a little more than high molecular polymer of mould simultaneously; 5) extrusion speed of pushing mechanism and the pulling speed of towing mechanism is set, and make pulling speed identical with extrusion speed, the homogeneity of structure composition during to ensure that chalcogenide glass is extruded is by the impact of gravity, then squeezing device is started, process furnace group heats container, makes the chalcogenide glass in container and polyphenylene sulfide be subject to thermal softening; Chalcogenide glass after softening and polyphenylene sulfide slowly, are equably extruded by pushing mechanism; The rod that extrudes extruded is brought down a fever through stove of bringing down a fever and is pulled device extraction; Labview programming software in conputer controlled platform reads and records squeeze and the time dependent data of extrusion temperature; 6) rod that extrudes of drawing is annealed after 6h under the transition temperature Tg of chalcogenide glass, then slow cooling is to room temperature; Namely the preform of embodiment four is obtained.
The chalcogenide glass fiber prefabricated rods of above-described embodiment one ~ embodiment four obtained, its structure composition evenly, surfaces externally and internally is smooth, interface is desirable, and top layer has the protective layer be made up 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 heating described container, 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 for annealing to the preform extruded, the bottom of 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 bring down a fever to be provided with between stove and described towing mechanism extrude the bending locating device of rod for preventing.
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, the first described process furnace is arranged on the top of described container, and the second described 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 control platform, the arranged outside of described container has temperature sensor, and described temperature sensor, the first described process furnace, the second described process furnace are all connected with described temperature control platform with described stove of bringing down a fever.
5. superposition method according to claim 4 extrudes the squeezing device of chalcogenide glass fiber prefabricated rods, it is characterized in that described extrusion stem is provided with pressure transmitter, 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, and it is characterized in that described pushing mechanism is provided with pressure warning unit, 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 conputer controlled platform, and described conputer controlled platform 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) get out chalcogenide glass and the high molecular polymer of polylith sheet, use alcohol rinse post-drying, put into vacuum vessel;
2) first a slice high molecular polymer is taken out, the chalcogenide glass of polylith sheet is superposed again successively on the top of this sheet high molecular polymer, then the high molecular polymer after superposition is put into container together with chalcogenide glass, and make high molecular polymer be placed on the lowermost end of container;
3) vacuum pump is utilized to vacuumize vacuum chamber, when the low vacuum of vacuum chamber is in 10
-2during Pa, topping up in vacuum chamber, makes the air pressure in vacuum chamber identical with external atmosphere pressure;
4) temperature control platform is opened, set process furnace group and the temperature of stove of bringing down a fever, and the temperature T setting mould is Tg<T<Tx, wherein Tx is the recrystallization temperature of chalcogenide glass, Tg is the transition temperature of chalcogenide glass, makes the softening temperature of temperature T a little more than high molecular polymer of mould simultaneously;
5) extrusion speed of pushing mechanism and the pulling speed of towing mechanism is set, and make pulling speed identical with extrusion speed, then start squeezing device, process furnace group heats container, makes the chalcogenide glass in container and high molecular polymer be subject to thermal softening; Chalcogenide glass after softening and high molecular polymer slowly, are equably extruded by pushing mechanism; The rod that extrudes extruded is brought down a fever through stove of bringing down a fever and is pulled device extraction;
6) extrude rod under the transition temperature Tg of chalcogenide glass after annealing 4 ~ 6h by what draw, then slow cooling is to room temperature; Namely chalcogenide glass fiber prefabricated rods is obtained.
10. superposition method according to claim 9 extrudes the method for chalcogenide glass fiber prefabricated rods, it is characterized in that the Δ T > 100 DEG C of described chalcogenide glass, wherein Δ T=Tx-Tg; Described high molecular polymer is any one in polyphenylene sulfide, polyimide and polysulfones; Described rare gas element is nitrogen or argon gas.
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| Application Number | Priority Date | Filing Date | Title |
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| 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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| 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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| CN103466933A CN103466933A (en) | 2013-12-25 |
| CN103466933B true CN103466933B (en) | 2015-10-28 |
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| 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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