CN112939444A - Extrusion preparation method of high polarization-maintaining microstructure optical fiber preform - Google Patents
Extrusion preparation method of high polarization-maintaining microstructure optical fiber preform Download PDFInfo
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- 239000013307 optical fiber Substances 0.000 title claims abstract description 150
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 239000000835 fiber Substances 0.000 claims abstract description 146
- 238000005253 cladding Methods 0.000 claims abstract description 96
- 239000011521 glass Substances 0.000 claims description 227
- 230000010287 polarization Effects 0.000 claims description 63
- 238000003825 pressing Methods 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 22
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- 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
- 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
- C03C13/00—Fibre or filament compositions
- C03C13/04—Fibre optics, e.g. core and clad fibre compositions
- C03C13/041—Non-oxide glass compositions
- C03C13/043—Chalcogenide glass compositions
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2203/00—Fibre product details, e.g. structure, shape
- C03B2203/30—Polarisation maintaining [PM], i.e. birefringent products, e.g. with elliptical core, by use of stress rods, "PANDA" type fibres
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Abstract
本发明涉及一种高保偏微结构光纤预制棒挤压制备方法，通过根据所要制备光纤预制棒的保偏微结构调整挤压腔的数量、挤压模的数量以及挤压模上的纤芯挤出孔形状，从而做出更多保偏微结构的光纤预制棒，进而加强了所得光纤预制棒的二阶对称性，由此得到具有更加稳定的纤芯‑包层比例、纤芯‑包层界面清晰完整且缺陷少以及具有更高保偏性能的光纤预制棒。
The invention relates to an extrusion preparation method for an optical fiber preform with a high polarization-maintaining microstructure. The number of extrusion cavities, the number of extrusion dies and the core extrusion on the extrusion die are adjusted according to the polarization-maintaining microstructure of the optical fiber preform to be prepared. The shape of the exit hole can be used to make more polarization-maintaining microstructure fiber preforms, thereby enhancing the second-order symmetry of the obtained fiber preforms, thereby obtaining a more stable core-cladding ratio, core-cladding ratio Optical fiber preform with clear and complete interface, less defects and higher polarization-maintaining performance.
Description
Technical Field
The invention relates to the field of optical fiber preforms, in particular to an extrusion preparation method of a high polarization maintaining microstructure optical fiber preform.
Background
As a special optical fiber among optical fibers, a polarization maintaining fiber is a special single mode optical fiber capable of allowing polarized light to transmit a long distance therein without changing the polarization state of the light. Therefore, polarization-maintaining optical fibers are also used in many fields requiring maintaining light polarization, such as sensors and optical fiber communication systems, because of their advantage of maintaining light polarization.
Polarization maintaining fibers generally fall into two categories: stress-type polarization-maintaining fibers and geometric-type polarization-maintaining fibers. The stress polarization-maintaining fiber introduces strong and fixed-direction stress inside the fiber, thereby weakening the influence of defects, residual stress and environmental stress on the polarization state of a light beam, and enabling the polarization state of the light beam to be maintained without change in the transmission process in the fiber. Stress type polarization maintaining optical fibers have the advantages of good longitudinal uniformity, excellent optical properties, high birefringence value, and the like, and are therefore one of the most commonly used types. However, the geometric polarization maintaining fiber has better temperature stability than the stress polarization maintaining fiber. Moreover, as the polarization maintaining performance of the geometric polarization maintaining optical fiber is mainly related to the optical fiber structure, the requirement of the preparation of the geometric polarization maintaining optical fiber on the experimental environment is relatively low.
The Chinese patent CN100592114C discloses a microstructure polarization maintaining fiber, which consists of a fiber core and a cladding, wherein the fiber core consists of a dielectric material 1 and periodically arranged holes 2, and when the cladding consists of only the dielectric material 3, the relations among refractive indexes n1, n2 and n3 of the dielectric material 1, the holes 2 and the dielectric material 3 are n1 > n3 > n2 or n2 > n3 > n 1; when the cladding is composed of the dielectric material 3 and the holes 4 periodically arranged in the dielectric material 3, the refractive indexes n1, n2, n3 and n4 of the dielectric material 1, the holes 2, the dielectric material 3 and the holes 4 are in the following relationship: n1 > n3 > n2 or n2 > n3 > n1 and n3 > n 4. That is, the granted patent CN100592114C is to make the core microstructured to have second-order symmetry, and to match the microstructured cladding, thereby realizing high polarization-maintaining performance of the optical fiber. However, the fiber core needs to be microstructured to make the fiber core have second-order symmetry, so that the preparation process for preparing the microstructure polarization-maintaining fiber is very complicated, and the microstructure fiber core needs to be stacked by a stacking method first, and then the stacked microstructure fiber core and the cladding are stacked into the fiber.
In addition, the invention patent CN105923988B issued in china discloses an extrusion preparation method of an elliptical core polarization maintaining optical fiber preform rod with arbitrarily adjustable ellipticity. The extrusion preparation method of the elliptical core polarization-maintaining optical fiber preform rod comprises two stages of staged extrusion, the prepared elliptical core polarization-maintaining optical fiber preform rod is high in size precision and has stable fiber core-cladding proportion, the ellipticity of a fiber core is basically consistent with that of an extrusion hole in a corresponding extrusion die, the fiber core is very close to a cladding in a fitting manner, and the fiber core-cladding interface is clear and complete; the method has good controllability, can accurately control the ellipticity of the fiber core of the elliptical core polarization maintaining optical fiber preform, overcomes the defect of structural defects of the elliptical core polarization maintaining optical fiber preform prepared by the traditional drilling or decompression burning shrinkage method, greatly reduces the cost compared with the traditional method for preparing the optical fiber preform by improving the chemical vapor deposition (MCVD), and solves the problem of poor fiber core-cladding interface of the elliptical core polarization maintaining optical fiber preform prepared by the traditional sleeving method. However, in the extrusion method for preparing the elliptical core polarization maintaining optical fiber preform of patent CN105923988B, the geometric structure of the prepared elliptical core polarization maintaining optical fiber preform is relatively simple, so that the polarization maintaining performance of the elliptical core polarization maintaining optical fiber finally obtained is poor.
Therefore, how to simply and conveniently prepare the optical fiber preform with high polarization maintaining performance becomes a technical problem which needs to be solved urgently in the field of the preparation of the optical fiber preform at present.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing a high polarization maintaining microstructure optical fiber preform by extrusion aiming at the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows: the extrusion preparation method of the high polarization maintaining microstructure optical fiber preform is characterized by comprising the following steps of:
step 4, putting each fiber core glass ingot into a corresponding extrusion cavity, putting each fiber core extrusion sheet into the corresponding extrusion cavity, and arranging each selected extrusion die at the bottom of the corresponding extrusion cavity; wherein, in the same extrusion cavity, the fiber core extrusion sheet is positioned above the fiber core glass ingot;
step 8, keeping the temperature in the extrusion cylinder unchanged at the preset temperature T, taking out the pressure applying head, placing each extrusion ejector rod into the extrusion cylinder, enabling the jacking end of each extrusion ejector rod to correspondingly penetrate through the radial through hole of the extrusion head and to be jacked and contacted with the upper surface of the fiber core extrusion piece in the corresponding extrusion cavity, then placing the pressure applying head again, and enabling the pressure applying head to be jacked and contacted with the stressed ends of all the extrusion ejector rods;
step 9, utilizing the pressure application head to apply pressure to all the extrusion ejector rods, enabling each extrusion ejector rod to apply top pressure to the fiber core extrusion sheet in the corresponding extrusion cavity, and extruding the fiber core glass in a softened state in the corresponding extrusion cavity from the fiber core extrusion holes of the corresponding extrusion die by each fiber core extrusion sheet to obtain a plurality of prefabricated rod fiber cores;
step 10, uniformly applying pressure to the fiber core glass in the softened state in each extrusion cavity and the cladding glass in the softened state in the extrusion cylinder, so that the fiber cores and the cladding glass of each prefabricated rod are extruded together at an extrusion opening of the extrusion cylinder to obtain a required initial product of the optical fiber prefabricated rod;
and 11, annealing the obtained optical fiber preform initial product at the transition temperature Tg for a preset time, and then cooling the temperature of the optical fiber preform initial product to room temperature to obtain the optical fiber preform product to be prepared.
In the method for preparing the high polarization maintaining microstructure optical fiber preform rod by extrusion, the extrusion cylinder, each extrusion cavity, the extrusion head, the pressure applying head, each extrusion ejector rod, each fiber core extrusion sheet and each extrusion die are subjected to ultrasonic cleaning and alcohol wiping treatment before use, and the fiber core glass ingot and the cladding glass ingot are washed by alcohol and deionized water before use.
And improving, wherein in the extrusion preparation method of the high polarization maintaining microstructure optical fiber preform, the steps 7 to 11 are all carried out in a vacuum environment of a vacuum cavity.
Further, in the extrusion preparation method of the high polarization maintaining microstructure optical fiber preform, the vacuum environment of the vacuum cavity is obtained by processing according to the following mode: vacuumizing the vacuum chamber by using a vacuum pump, so that the vacuum degree in the vacuum chamber is lower than 10-2And when Pa is needed, supplementing inert gas into the vacuum cavity to enable the air pressure in the vacuum cavity to be the same as the external atmospheric pressure.
In the extrusion preparation method of the high polarization maintaining microstructure optical fiber preform, the shapes of the fiber core extrusion holes of the extrusion dies in the extrusion die set are not completely the same.
In the extrusion preparation method of the high polarization maintaining microstructure optical fiber preform, each extrusion cavity is detachably fastened at the bottom of an extrusion head.
Further improved, in the extrusion preparation method of the high polarization maintaining microstructure optical fiber preform, the preset time in the step 11 is 4-12 hours.
And improving the method, wherein in the extrusion preparation method of the high polarization maintaining microstructure optical fiber preform, each fiber core glass ingot and each cladding glass ingot are chalcogenide glass ingots.
Further, in the extrusion preparation method of the high polarization maintaining microstructure optical fiber preform, the fiber core glass ingot is Ge9As23Se68The clad glass ingot is Ge10As22Se68。
Compared with the prior art, the invention has the advantages that:
firstly, compared with the traditional stacking preparation method, the extrusion preparation method of the high polarization-maintaining microstructure optical fiber preform rod provided by the invention has a simple preparation process, the finally obtained optical fiber preform rod product has a more stable fiber core-cladding ratio, the fiber core and the cladding are more tightly attached, the fiber core-cladding interface is clear and complete, the defects are few, and the prepared optical fiber preform rod product can well ensure the second-order symmetry;
secondly, the extrusion preparation method of the high polarization-maintaining microstructure optical fiber preform has better controllability, so that the purity of fiber core components can be ensured, and the defect that the surface of the fiber core is easily oxidized and polluted when the traditional stacking preparation method is adopted is effectively overcome; in addition, by replacing glass components meeting the optical and thermal matching requirements, the high polarization maintaining performance microstructure optical fiber prefabricated rod with different performances can be prepared;
in addition, the extrusion preparation method of the high polarization-maintaining microstructure optical fiber preform rod can also adjust the number of the extrusion dies and the shapes of fiber core extrusion holes of the extrusion dies according to the polarization-maintaining microstructure of the optical fiber preform rod to be prepared, so that optical fiber preform rods with more structures can be prepared, the second-order symmetry of the obtained optical fiber preform rod is further enhanced, and the polarization-maintaining performance of the obtained optical fiber preform rod is further improved;
finally, in the extrusion preparation method of the high polarization maintaining microstructure optical fiber preform rod, the bottom of the pressure applying head applies surface pressure to the whole plane at the top of the extrusion head, so that not only can the damage of a mold caused by applying pressure to the central point of the extrusion head by a traditional extrusion rod be reduced, but also the problem of micro-angle inclination of the extrusion head and an extrusion cavity when extruding cladding glass due to uneven stress caused by applying pressure to the traditional point can be effectively avoided;
in addition, when the cladding glass at the bottom of the extrusion cylinder is extruded, the extrusion head does not apply extrusion force to the cladding glass, the softened cladding glass is driven to be extruded out of the extrusion opening through the flow of the fiber core, and the pressure data reflected by the pressure gauge is only the pressure of the fiber core glass, so that the softened state of the fiber core glass in the extrusion cavity can be more accurately pushed out of the pressure gauge, the heating temperature in the extrusion cylinder can be more accurately controlled, the fiber core glass can reach the proper softened state, and the shape of the fiber core can be better controlled.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing a high polarization maintaining microstructure optical fiber preform by extrusion according to the present invention;
FIG. 2 is a schematic diagram of an extrusion chamber before being extruded by an extrusion head according to a first embodiment of the present invention;
FIG. 3 is a schematic diagram illustrating the extrusion chamber at the end of extrusion by the pressure application head according to the first embodiment of the present invention;
FIG. 4 is a schematic view of a state in which the pressing head touches the force-bearing ends of all the pressing rams in the first embodiment of the present invention;
FIG. 5 is a schematic view showing a state where the pressing of each of the core glass and the clad glass is terminated in the first embodiment of the present invention;
FIG. 6 is a schematic cross-sectional view of an optical fiber preform product obtained in a first embodiment of the present invention;
FIG. 7 is a schematic cross-sectional view of an optical fiber preform product obtained in the second example of the present invention;
FIG. 8 is a schematic diagram of the extrusion chamber of the third embodiment of the present invention before being extruded by the extrusion head;
FIG. 9 is a schematic view showing the state of the extrusion chamber at the end of extrusion by the pressure application head in the third embodiment of the present invention;
FIG. 10 is a schematic view of the third embodiment of the present invention, wherein the pressing head touches the force-bearing ends of all the pressing rams;
FIG. 11 is a diagram showing a state where the pressing of each of the core glass and the clad glass is terminated in the third embodiment of the present invention;
FIG. 12 is a schematic cross-sectional view of an optical fiber preform product obtained in the third example of the present invention.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
Example one
In the first embodiment, the high polarization maintaining microstructure optical fiber preform to be prepared is set as a chalcogenide optical fiber preform, and the core glass ingot selected for use is Ge9As23Se68The cladding glass ingot is Ge10As22Se68Here, the high polarization maintaining microstructure is a bow tie-like polarization maintaining structure. Specifically, the extrusion preparation method of the high polarization maintaining microstructure chalcogenide optical fiber preform in the embodiment includes the following steps:
wherein, the extrusion container 1, each extrusion cavity 2, the extrusion head 3, the pressure applying head 4, each extrusion mandril 5, each fiber core extrusion sheet 21 and each extrusion die 22 prepared in the step 1 are all subjected to ultrasonic cleaning and alcohol wiping treatment before use;
the outer diameter of the extrusion head 3 and the outer diameter of the pressure applying head 4 are set to be slightly smaller than the size of an upper opening 11 of the extrusion container 1, so that the extrusion head 3 and the pressure applying head 4 can be placed into the inner side of the extrusion container 1 through the upper opening 11, gaps are formed between the extrusion head 3 and the inner wall of the extrusion container and between the pressure applying head 4 and the inner wall of the extrusion container at the moment, and the extrusion head 3 and the pressure applying head 4 can move in the extrusion container 1; of course, it is preferable that the outer diameter of the extrusion head 3 is closely attached to the inner sidewall of the container 1 and the extrusion head 3 can move up and down in the container 1; in this way, it can be ensured that each extrusion cavity 2 can receive more uniform downward extrusion force applied to the extrusion head 3 by the pressure applying head 4 in the subsequent process of extruding each extrusion cavity 2 by the pressure applying head 4;
referred to herein as Ge9As23Se68The outer diameter of the core glass ingot 6 is matched with the inner diameter of the extrusion cavity 2, namely Ge9As23Se68The core glass ingot 6 can be placed just inside the extrusion chamber 2 and Ge9As23Se68The fiber core glass ingot 6 can be tightly attached to the inner side wall of the extrusion cavity 2; and, Ge10As22Se68The clad glass ingot 7 can be placed just inside the container 1 and Ge10As22Se68The cladding glass ingot 7 can be tightly attached to the inner side wall of the extrusion container 1;
in addition, in this step 3, Ge9As23Se68 Core glass ingot 6 and Ge10As22Se68The cladding glass ingot 7 is subjected to ultrasonic cleaning and alcohol wiping treatment before use to remove impurities on the surfaces of two chalcogenide glass ingots, so that adverse effects of the impurities on the preparation of the optical fiber preform by subsequent extrusion are avoided; of course, when the glass ingots are cleaned by ultrasonic waves and treated by alcohol, the glass ingots can be further cleaned by distilled water or deionized water;
step 4, adding Ge9As23Se68Putting the fiber core glass ingot 6 into the corresponding extrusion cavity 2, putting each fiber core extrusion sheet 21 into the corresponding extrusion cavity 2, and arranging each selected extrusion die 22 at the bottom of the corresponding extrusion cavity 2; wherein, in the same extrusion cavity 2, the fiber core extrusion sheet 21 is positioned in Ge9As23Se68Above the core glass ingot 6; the extrusion cavity 2 can protect Ge9As23Se68 Core glass ingot 6, ensuring that it can be integrally squeezed into the softened Ge10As22Se68 Clad glass ingot 7;
step 8, keeping the temperature in the extrusion cylinder 1 unchanged at a preset temperature T (namely 200 ℃), taking out the pressure applying head 4, putting each extrusion ejector rod 5 into the extrusion cylinder 1, enabling the jacking end of each extrusion ejector rod 5 to correspondingly penetrate through the radial through hole 30 of the extrusion head 3 and to be jacked and contacted with the upper surface of the fiber core extrusion sheet 21 in the corresponding extrusion cavity 2, then putting the pressure applying head 4 again, and enabling the pressure applying head 4 to be jacked and contacted with the stressed ends of all the extrusion ejector rods 5; wherein, the state when the pressure applying head 4 pushes against the stress ends of all the extrusion mandrils 5 is shown in figure 4;
furthermore, byIn Ge9As23Se68The outer diameter of the fiber core glass ingot 6 is matched with the inner diameter of the extrusion cavity 2, so that when the pressing head 4 is taken out and disassembled and the extrusion mandril 5 is replaced, when the extrusion mandril 5 is extruded, the inside of the extrusion cavity 2 can prevent the glass on the inner side from flowing upwards under the action of pressure, and the smooth extrusion process is ensured;
step 9, utilizing the pressure applying head 4 to apply pressure to all the extrusion ejector rods 5, enabling each extrusion ejector rod 5 to apply top pressure to the fiber core extrusion sheets 21 in the corresponding extrusion cavity 2, and enabling each fiber core extrusion sheet 21 to apply softened Ge in the corresponding extrusion cavity 29As23Se68The core glass is extruded from the corresponding core extrusion holes 220 of the extrusion die 22 to obtain a plurality of preform cores; wherein the diameter of the core of the extruded preform is smaller than the corresponding Ge9As23Se68The diameter of the core glass;
step 10, softening Ge in each extrusion cavity 29As23Se68Core glass and Ge in softened state in extrusion container 110As22Se68The cladding glass is uniformly pressed to make each prefabricated rod fiber core and Ge10As22Se68The clad glass is extruded together at an extrusion opening 12 of the extrusion cylinder 1 to obtain a required initial product of the optical fiber perform; wherein for each Ge9As23Se68Core glass and Ge10As22Se68The state of the clad glass at the end of pressing is shown in FIG. 5; due to the portion of Ge extruded by the extrusion ram 59As23Se68 Core glass ingot 6 is in Ge9As23Se68 Core glass ingot 6 and Ge10As22Se68The clad glass ingot 7 is internally penetrated so that the portion of the Ge being pressed can be prevented from being pressed9As23Se68The core glass ingot 6 is adversely affected by impurities such as oxygen outside the extrusion chamber 2 and the extrusion barrel 1, and the Ge content of the core of the optical fiber preform obtained subsequently is increased9As23Se68The purity of the fiber core glass ingot 6 is improved, and then the purity of the fiber core of the obtained optical fiber preform is improved;
in this step 10, Ge in a softened state is provided in each extrusion chamber 29As23Se68Core glass and Ge in softened state in extrusion container 110As22Se68The cladding glass is uniformly pressed, so that the purity uniformity of the initial product of the obtained optical fiber perform and the purity uniformity of the subsequent finally obtained optical fiber perform can be improved, the occurrence of a fracture phenomenon caused by the uneven speed of the initial product of the prepared optical fiber perform and the subsequent finally obtained optical fiber perform can be avoided, and the product quality of the prepared optical fiber perform is improved;
and 11, annealing the obtained optical fiber perform initial product at the transition temperature Tg for a preset time, and then cooling the temperature of the optical fiber perform initial product to room temperature to obtain the optical fiber perform product to be prepared. Wherein the preset time is set to be 4-12 h.
The extruded optical fiber preform product was observed under a microscope, and the cross section of the obtained optical fiber preform product was shown in FIG. 6. In fig. 6, reference numeral 00 denotes a circular core glass of the obtained optical fiber preform product, reference numeral 01 denotes a core glass of the similar bow tie shape of the obtained optical fiber preform product, and reference numeral 02 denotes a cladding glass of the obtained optical fiber preform product. As can be seen from fig. 6, the shape of the fiber core is substantially consistent with the shape of the fiber core extrusion hole on the corresponding extrusion die, in the obtained optical fiber preform product, the fiber core and the cladding of the optical fiber preform are very tightly attached, the fiber core-cladding interface is clear and complete, and the problem of poor fiber core-cladding interface of the preform prepared by the traditional extrusion preparation method does not exist, so that the optical fiber preform prepared in the embodiment has higher dimensional accuracy. In addition, the chalcogenide optical fiber preform prepared by adopting the chalcogenide material in the embodiment has a high polarization maintaining microstructure, has the advantages of better mechanical property and physical and chemical stability of chalcogenide glass optical fibers and the like, and effectively improves the overall performance of the chalcogenide optical fiber preform.
Example two
In the second embodiment, letThe high polarization maintaining microstructure optical fiber preform to be prepared is determined to be a chalcogenide optical fiber preform, and the selected fiber core glass ingot is Ge9As23Se68The cladding glass ingot is Ge10As22Se68Here, the high polarization maintaining microstructure is a panda-type polarization maintaining structure. Specifically, the extrusion preparation method of the high polarization maintaining microstructure chalcogenide optical fiber preform in the embodiment includes the following steps:
step 1, preparing an extrusion container 1, three extrusion cavities 2, an extrusion head 3, a pressure applying head 4 and three extrusion mandrils 5 in advance; the top of the extrusion container 1 is provided with an upper opening 11, the bottom of the extrusion container 1 is provided with an extrusion opening 12, and the outer diameter of the extrusion head 3 and the outer diameter of the pressure applying head 4 are both slightly smaller than the size of the upper opening 11 of the extrusion container 1; each extrusion cavity 2 is detachably arranged in the extrusion container 1, and each extrusion cavity 2 is detachably fastened at the bottom of the extrusion head 3; the extrusion cavity 2 is provided with a top opening and a bottom opening, a fiber core extrusion sheet 21 capable of moving back and forth along the axial direction of the extrusion cavity 2 is detachably arranged in the extrusion cavity 2, an extrusion die 22 is arranged at the bottom of the extrusion cavity 2, the extrusion die 22 seals the bottom opening of the extrusion cavity 2, and a fiber core extrusion hole 220 communicated with the inner side of the extrusion cavity 2 is formed in the extrusion die 22; the extrusion head 3 is provided with three radial through holes 30 which are in one-to-one correspondence with the centers of the top openings of the extrusion cavities 2, the radial through holes 30 are in one-to-one correspondence with the extrusion ejector rods 5, and each extrusion ejector rod 5 can move back and forth in the corresponding radial through hole 30;
wherein, the extrusion container 1, each extrusion cavity 2, the extrusion head 3, the pressure applying head 4, each extrusion mandril 5, each fiber core extrusion sheet 21 and each extrusion die 22 prepared in the step 1 are all subjected to ultrasonic cleaning and alcohol wiping treatment before use;
the outer diameter of the extrusion head 3 and the outer diameter of the pressure applying head 4 are set to be slightly smaller than the size of an upper opening 11 of the extrusion container 1, so that the extrusion head 3 and the pressure applying head 4 can be placed into the inner side of the extrusion container 1 through the upper opening 11, gaps are formed between the extrusion head 3 and the inner wall of the extrusion container and between the pressure applying head 4 and the inner wall of the extrusion container at the moment, and the extrusion head 3 and the pressure applying head 4 can move in the extrusion container 1; of course, it is preferable that the outer diameter of the extrusion head 3 is closely attached to the inner sidewall of the container 1 and the extrusion head 3 can move up and down in the container 1; in this way, it can be ensured that each extrusion cavity 2 can receive more uniform downward extrusion force applied to the extrusion head 3 by the pressure applying head 4 in the subsequent process of extruding each extrusion cavity 2 by the pressure applying head 4;
referred to herein as Ge9As23Se68The outer diameter of the core glass ingot 6 is matched with the inner diameter of the extrusion cavity 2, namely Ge9As23Se68The core glass ingot 6 can be placed just inside the extrusion chamber 2 and Ge9As23Se68The fiber core glass ingot 6 can be tightly attached to the inner side wall of the extrusion cavity 2; and, Ge10As22Se68The clad glass ingot 7 can be placed just inside the container 1 and Ge10As22Se68The cladding glass ingot 7 can be tightly attached to the inner side wall of the extrusion container 1;
in addition, in this step 3, Ge9As23Se68 Core glass ingot 6 and Ge10As22Se68 Clad glass ingot 7 before useUltrasonic cleaning and alcohol wiping are carried out to remove impurities on the surfaces of two chalcogenide glass ingots, so that adverse effects of the impurities on the preparation of the optical fiber preform by subsequent extrusion are avoided; of course, when the glass ingots are cleaned by ultrasonic waves and treated by alcohol, the glass ingots can be further cleaned by distilled water or deionized water;
step 4, adding Ge9As23Se68Putting the fiber core glass ingot 6 into the corresponding extrusion cavity 2, putting each fiber core extrusion sheet 21 into the corresponding extrusion cavity 2, and arranging each selected extrusion die 22 at the bottom of the corresponding extrusion cavity 2; wherein, in the same extrusion cavity 2, the fiber core extrusion sheet 21 is positioned in Ge9As23Se68Above the core glass ingot 6; the extrusion cavity 2 can protect Ge9As23Se68 Core glass ingot 6, ensuring that it can be integrally squeezed into the softened Ge10As22Se68 Clad glass ingot 7;
step 8, keeping the temperature in the extrusion cylinder 1 unchanged at a preset temperature T (namely 200 ℃), taking out the pressure applying head 4, putting each extrusion ejector rod 5 into the extrusion cylinder 1, enabling the jacking end of each extrusion ejector rod 5 to correspondingly penetrate through the radial through hole 30 of the extrusion head 3 and to be jacked and contacted with the upper surface of the fiber core extrusion sheet 21 in the corresponding extrusion cavity 2, then putting the pressure applying head 4 again, and enabling the pressure applying head 4 to be jacked and contacted with the stressed ends of all the extrusion ejector rods 5; wherein, the state when the pressure applying head 4 pushes against the force bearing ends of all the extrusion mandrils 5 is similar to that shown in figure 4 in the first embodiment;
in addition, due to Ge9As23Se68Outer diameter of core glass ingot 6 andthe inner diameter of the extrusion cavity 2 is matched, so that when the pressing head 4 is taken out and disassembled and the extrusion mandril 5 is replaced, when the extrusion mandril 5 is extruded, the inside of the extrusion cavity can prevent the glass at the inner side from flowing upwards in a reverse direction under the action of pressure, and the smooth operation of the extrusion process is ensured;
step 9, utilizing the pressure applying head 4 to apply pressure to all the extrusion ejector rods 5, enabling each extrusion ejector rod 5 to apply top pressure to the fiber core extrusion sheets 21 in the corresponding extrusion cavity 2, and enabling each fiber core extrusion sheet 21 to apply softened Ge in the corresponding extrusion cavity 29As23Se68The core glass is extruded from the corresponding core extrusion holes 220 of the extrusion die 22 to obtain a plurality of preform cores; wherein the diameter of the core of the extruded preform is smaller than the corresponding Ge9As23Se68The diameter of the core glass;
step 10, softening Ge in each extrusion cavity 29As23Se68Core glass and Ge in softened state in extrusion container 110As22Se68The cladding glass is uniformly pressed to make each prefabricated rod fiber core and Ge10As22Se68The clad glass is extruded together at an extrusion opening 12 of the extrusion cylinder 1 to obtain a required initial product of the optical fiber perform; wherein for each Ge9As23Se68Core glass and Ge10As22Se68The state of the clad glass at the end of pressing is similar to that shown in FIG. 5 in the first embodiment; due to the portion of Ge extruded by the extrusion ram 59As23Se68 Core glass ingot 6 is in Ge9As23Se68 Core glass ingot 6 and Ge10As22Se68The clad glass ingot 7 is internally penetrated so that the portion of the Ge being pressed can be prevented from being pressed9As23Se68The core glass ingot 6 is adversely affected by impurities such as oxygen outside the extrusion chamber 2 and the extrusion barrel 1, and the Ge content of the core of the optical fiber preform obtained subsequently is increased9As23Se68The purity of the fiber core glass ingot 6 is improved, and then the purity of the fiber core of the obtained optical fiber preform is improved;
in this step 10, each extrusion is setGe in softened state in the cavity 29As23Se68Core glass and Ge in softened state in extrusion container 110As22Se68The cladding glass is uniformly pressed, so that the purity uniformity of the initial product of the obtained optical fiber perform and the purity uniformity of the subsequent finally obtained optical fiber perform can be improved, the occurrence of a fracture phenomenon caused by the uneven speed of the initial product of the prepared optical fiber perform and the subsequent finally obtained optical fiber perform can be avoided, and the product quality of the prepared optical fiber perform is improved;
and 11, annealing the obtained optical fiber preform initial product at the transition temperature Tg for a preset time period, and then cooling the temperature of the optical fiber preform initial product to room temperature to obtain the optical fiber preform product to be prepared. Wherein the preset time is set to be 4-12 h.
The extruded optical fiber preform product was observed under a microscope, and the cross section of the resulting optical fiber preform product was shown in FIG. 7. In fig. 7, reference numeral 01 denotes a circular core glass of the obtained optical fiber preform product, two reference numerals 03 denote two large circular core glasses of the obtained optical fiber preform product, and reference numeral 02 denotes a cladding glass of the obtained optical fiber preform product. As can be seen from fig. 7, the shape of the fiber core is substantially consistent with the shape of the fiber core extrusion hole on the corresponding extrusion die, in the obtained optical fiber preform product, the fiber core and the cladding of the optical fiber preform are very tightly attached, the fiber core-cladding interface is clear and complete, and the problem of poor fiber core-cladding interface of the preform prepared by the traditional extrusion preparation method does not exist, so that the optical fiber preform prepared in the embodiment has higher dimensional accuracy. In addition, the chalcogenide optical fiber preform prepared by adopting the chalcogenide material in the embodiment has a high polarization maintaining microstructure, has the advantages of better mechanical property and physical and chemical stability of chalcogenide glass optical fibers and the like, and effectively improves the overall performance of the chalcogenide optical fiber preform.
EXAMPLE III
In the third embodiment, the high polarization maintaining microstructure optical fiber preform to be prepared is setFor chalcogenide preforms, the core glass ingot chosen for use is Ge9As23Se68The cladding glass ingot is Ge10As22Se68Here, the high polarization maintaining microstructure is a linear five-core polarization maintaining structure. Specifically, the extrusion preparation method of the high polarization maintaining microstructure chalcogenide optical fiber preform in the embodiment includes the following steps:
step 1, preparing an extrusion container 1, five extrusion cavities 2, an extrusion head 3, a pressure applying head 4 and five extrusion mandrils 5 in advance; the top of the extrusion container 1 is provided with an upper opening 11, the bottom of the extrusion container 1 is provided with an extrusion opening 12, and the outer diameter of the extrusion head 3 and the outer diameter of the pressure applying head 4 are both slightly smaller than the size of the upper opening 11 of the extrusion container 1; each extrusion cavity 2 is detachably arranged in the extrusion container 1, and each extrusion cavity 2 is detachably fastened at the bottom of the extrusion head 3; the extrusion cavity 2 is provided with a top opening 21 and a bottom opening 22, a fiber core extrusion sheet 21 capable of moving back and forth along the axial direction of the extrusion cavity 2 is detachably arranged in the extrusion cavity 2, an extrusion die 22 is arranged at the bottom of the extrusion cavity 2, the extrusion die 22 seals the bottom opening 22 of the extrusion cavity 2, and a fiber core extrusion hole 220 communicated with the inner side of the extrusion cavity 2 is formed in the extrusion die 22; the extrusion head 3 is provided with five radial through holes 30 which are in one-to-one correspondence with the centers of the top openings of the extrusion cavities 2, the radial through holes 30 are in one-to-one correspondence with the extrusion ejector rods 5, and each extrusion ejector rod 5 can move back and forth in the corresponding radial through hole 30;
wherein, the extrusion container 1, each extrusion cavity 2, the extrusion head 3, the pressure applying head 4, each extrusion mandril 5, each fiber core extrusion sheet 21 and each extrusion die 22 prepared in the step 1 are all subjected to ultrasonic cleaning and alcohol wiping treatment before use;
the outer diameter of the extrusion head 3 and the outer diameter of the pressure applying head 4 are set to be slightly smaller than the size of an upper opening 11 of the extrusion container 1, so that the extrusion head 3 and the pressure applying head 4 can be placed into the inner side of the extrusion container 1 through the upper opening 11, gaps are formed between the extrusion head 3 and the inner wall of the extrusion container and between the pressure applying head 4 and the inner wall of the extrusion container at the moment, and the extrusion head 3 and the pressure applying head 4 can move in the extrusion container 1; of course, it is preferable that the outer diameter of the extrusion head 3 is closely attached to the inner sidewall of the container 1 and the extrusion head 3 can move up and down in the container 1; in this way, it can be ensured that each extrusion cavity 2 can receive more uniform downward extrusion force applied to the extrusion head 3 by the pressure applying head 4 in the subsequent process of extruding each extrusion cavity 2 by the pressure applying head 4;
referred to herein as Ge9As23Se68The outer diameter of the core glass ingot 6 is matched with the inner diameter of the extrusion cavity 2, namely Ge9As23Se68The core glass ingot 6 can be placed just inside the extrusion chamber 2 and Ge9As23Se68The fiber core glass ingot 6 can be tightly attached to the inner side wall of the extrusion cavity 2; and, Ge10As22Se68The clad glass ingot 7 can be placed just inside the container 1 and Ge10As22Se68The cladding glass ingot 7 can be tightly attached to the inner side wall of the extrusion container 1;
in addition, in this step 3, Ge9As23Se68 Core glass ingot 6 and Ge10As22Se68The cladding glass ingot 7 is cleaned by ultrasonic wave and wiped by alcohol before useThe purification treatment is carried out to remove impurities on the surfaces of the two chalcogenide glass ingots and avoid the impurities from causing adverse effects on the preparation of the optical fiber preform by subsequent extrusion; of course, when the glass ingots are cleaned by ultrasonic waves and treated by alcohol, the glass ingots can be further cleaned by distilled water or deionized water;
step 4, adding Ge9As23Se68Putting the fiber core glass ingot 6 into the corresponding extrusion cavity 2, putting each fiber core extrusion sheet 21 into the corresponding extrusion cavity 2, and arranging each selected extrusion die 22 at the bottom of the corresponding extrusion cavity 2; wherein, in the same extrusion cavity 2, the fiber core extrusion sheet 21 is positioned in Ge9As23Se68Above the core glass ingot 6; the extrusion cavity 2 can protect Ge9As23Se68 Core glass ingot 6, ensuring that it can be integrally squeezed into the softened Ge10As22Se68 Clad glass ingot 7;
step 8, keeping the temperature in the extrusion cylinder 1 unchanged at a preset temperature T (namely 200 ℃), taking out the pressure applying head 4, putting each extrusion ejector rod 5 into the extrusion cylinder 1, enabling the jacking end of each extrusion ejector rod 5 to correspondingly penetrate through the radial through hole 30 of the extrusion head 3 and to be jacked and contacted with the upper surface of the fiber core extrusion sheet 21 in the corresponding extrusion cavity 2, then putting the pressure applying head 4 again, and enabling the pressure applying head 4 to be jacked and contacted with the stressed ends of all the extrusion ejector rods 5; the state of the pressing head 4 contacting the force bearing ends of all the extrusion mandrils 5 is shown in figure 10;
in addition, due to Ge9As23Se68The outer diameter of the core glass ingot 6 is adapted to the inner diameter of the extrusion chamber 2, so that the extrusion head 4 is removed and the extrusion ram 5 is replacedWhen the extrusion mandril 5 is extruded, the glass inside the extrusion cavity 2 can be prevented from flowing upwards in the reverse direction under the action of pressure, so that the smooth operation of the extrusion process is ensured;
step 9, utilizing the pressure applying head 4 to apply pressure to all the extrusion ejector rods 5, enabling each extrusion ejector rod 5 to apply top pressure to the fiber core extrusion sheets 21 in the corresponding extrusion cavity 2, and enabling each fiber core extrusion sheet 21 to apply softened Ge in the corresponding extrusion cavity 29As23Se68The core glass is extruded from the corresponding core extrusion holes 220 of the extrusion die 22 to obtain a plurality of preform cores; wherein the diameter of the core of the extruded preform is smaller than the corresponding Ge9As23Se68The diameter of the core glass;
step 10, softening Ge in each extrusion cavity 29As23Se68Core glass and Ge in softened state in extrusion container 110As22Se68The cladding glass is uniformly pressed to make each prefabricated rod fiber core and Ge10As22Se68The clad glass is extruded together at an extrusion opening 12 of the extrusion cylinder 1 to obtain a required initial product of the optical fiber perform; wherein for each Ge9As23Se68Core glass and Ge10As22Se68The state when the pressing of the clad glass is finished is shown in FIG. 11; due to the portion of Ge extruded by the extrusion ram 59As23Se68 Core glass ingot 6 is in Ge9As23Se68 Core glass ingot 6 and Ge10As22Se68The clad glass ingot 7 is internally penetrated so that the portion of the Ge being pressed can be prevented from being pressed9As23Se68The core glass ingot 6 is adversely affected by impurities such as oxygen outside the extrusion chamber 2 and the extrusion barrel 1, and the Ge content of the core of the optical fiber preform obtained subsequently is increased9As23Se68The purity of the fiber core glass ingot 6 is improved, and then the purity of the fiber core of the obtained optical fiber preform is improved;
in this step 10, Ge in a softened state is provided in each extrusion chamber 29As23Se68Core glass and in softened state in extrusion cylinderGe10As22Se68The cladding glass is uniformly pressed, so that the purity uniformity of the initial product of the obtained optical fiber perform and the purity uniformity of the subsequent finally obtained optical fiber perform can be improved, the occurrence of a fracture phenomenon caused by the uneven speed of the initial product of the prepared optical fiber perform and the subsequent finally obtained optical fiber perform can be avoided, and the product quality of the prepared optical fiber perform is improved;
and 11, annealing the obtained optical fiber preform initial product at the transition temperature Tg for a preset time period, and then cooling the temperature of the optical fiber preform initial product to room temperature to obtain the optical fiber preform product to be prepared. Wherein the preset time is set to be 4-12 h.
The extruded optical fiber preform product was observed under a microscope, and the cross section of the obtained optical fiber preform product was shown in FIG. 12. In fig. 12, reference numeral 01 denotes a circular core glass of the obtained optical fiber preform product, four reference numerals 03 denote four large circular core glasses of the obtained optical fiber preform product, and reference numeral 02 denotes a cladding glass of the obtained optical fiber preform product. As can be seen from fig. 12, the shape of the fiber core is substantially consistent with the shape of the fiber core extrusion hole on the corresponding extrusion die, in the obtained optical fiber preform product, the fiber core and the cladding of the optical fiber preform are very tightly attached, the fiber core-cladding interface is clear and complete, and the problem of poor fiber core-cladding interface of the preform prepared by the conventional extrusion preparation method does not exist, so that the optical fiber preform prepared in the embodiment has higher dimensional accuracy. In addition, the chalcogenide optical fiber preform prepared by adopting the chalcogenide material in the embodiment has a high polarization maintaining microstructure, has the advantages of better mechanical property and physical and chemical stability of chalcogenide glass optical fibers and the like, and effectively improves the overall performance of the chalcogenide optical fiber preform.
Although preferred embodiments of the present invention have been described in detail hereinabove, it should be clearly understood that modifications and variations of the present invention are possible to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The extrusion preparation method of the high polarization maintaining microstructure optical fiber preform is characterized by comprising the following steps of:
step 1, preparing an extrusion container, a plurality of extrusion cavities, an extrusion head, a pressure applying head and a plurality of extrusion ejector rods in advance; the top of the extrusion cylinder is provided with an upper opening, the bottom of the extrusion cylinder is provided with an extrusion opening, and the outer diameter of the extrusion head and the outer diameter of the pressure application head are both smaller than the size of the upper opening of the extrusion cylinder; each extrusion cavity is detachably arranged in the extrusion container, the extrusion cavity is provided with a top opening and a bottom opening, a fiber core extrusion sheet capable of moving back and forth along the axial direction of the extrusion cavity is detachably arranged in the extrusion cavity, the bottom of the extrusion cavity is provided with an extrusion die, the bottom opening of the extrusion cavity is blocked by the extrusion die, and a fiber core extrusion hole communicated with the inner side of the extrusion cavity is formed in the extrusion die; the extrusion head is provided with a plurality of radial through holes which are in one-to-one correspondence with the centers of the top openings of the extrusion cavities, the radial through holes are in one-to-one correspondence with the extrusion ejector rods, and each extrusion ejector rod can move back and forth in the corresponding radial through hole;
step 2, selecting an extrusion head and an extrusion module corresponding to the polarization maintaining microstructure of the optical fiber preform to be prepared; wherein the extrusion module is provided with a plurality of extrusion dies;
step 3, respectively preparing cleaned and dried fiber core glass ingots and cladding glass ingots; the number of the fiber core glass ingots is equal to that of the extrusion cavities, and the fiber core glass ingots correspond to the extrusion cavities one by one; the outer diameter of each fiber core glass ingot is matched with the inner diameter of the corresponding extrusion cavity, and the outer diameter of the cladding glass ingot is matched with the inner diameter of the extrusion cylinder;
step 4, putting each fiber core glass ingot into a corresponding extrusion cavity, putting each fiber core extrusion sheet into the corresponding extrusion cavity, and arranging each selected extrusion die at the bottom of the corresponding extrusion cavity; wherein, in the same extrusion cavity, the fiber core extrusion sheet is positioned above the fiber core glass ingot;
step 5, placing the cladding glass ingot at the bottom of an extrusion container, then placing all the assembled extrusion cavities and extrusion heads in the extrusion container, enabling the extrusion heads to be propped against the tops of all the extrusion cavities, enabling the bottoms of the pressure applying heads to be propped against the whole plane of the tops of the extrusion heads, and enabling the centers of the pressure applying heads and the extrusion heads to be positioned on the same straight line; wherein each extrusion cavity is positioned above a cladding glass ingot in the extrusion cylinder;
step 6, heating the extrusion container with the extrusion cavity and the cladding glass ingot, and heating the temperature in the extrusion container to a preset temperature T, so that all the fiber core glass ingots and the cladding glass ingots in the extrusion container are heated and softened, and fiber core glass in a softened state and cladding glass in a softened state are obtained; wherein the preset temperature T satisfies: tg < T < Tx, wherein Tg is the maximum value of the transition temperature of the core glass and the transition temperature of the cladding glass, and Tx is the minimum value of the crystallization temperature of the core glass and the crystallization temperature of the cladding glass;
step 7, pressing the top of the extrusion head by using a pressing head, and pushing each extrusion cavity into the cladding glass in a softened state by using the extrusion head so that the bottom of each extrusion cavity is flush with the bottom of the cladding glass;
step 8, keeping the temperature in the extrusion cylinder unchanged at the preset temperature T, taking out the pressure applying head, placing each extrusion ejector rod into the extrusion cylinder, enabling the jacking end of each extrusion ejector rod to correspondingly penetrate through the radial through hole of the extrusion head and to be jacked and contacted with the upper surface of the fiber core extrusion piece in the corresponding extrusion cavity, then placing the pressure applying head again, and enabling the pressure applying head to be jacked and contacted with the stressed ends of all the extrusion ejector rods;
step 9, utilizing the pressure application head to apply pressure to all the extrusion ejector rods, enabling each extrusion ejector rod to apply top pressure to the fiber core extrusion sheet in the corresponding extrusion cavity, and extruding the fiber core glass in a softened state in the corresponding extrusion cavity from the fiber core extrusion holes of the corresponding extrusion die by each fiber core extrusion sheet to obtain a plurality of prefabricated rod fiber cores;
step 10, uniformly applying pressure to the fiber core glass in the softened state in each extrusion cavity and the cladding glass in the softened state in the extrusion cylinder, so that the fiber cores and the cladding glass of each prefabricated rod are extruded together at an extrusion opening of the extrusion cylinder to obtain a required initial product of the optical fiber prefabricated rod;
and 11, annealing the obtained optical fiber preform initial product at the transition temperature Tg for a preset time, and then cooling the temperature of the optical fiber preform initial product to room temperature to obtain the optical fiber preform product to be prepared.
2. The extrusion method for preparing a high polarization maintaining microstructure optical fiber preform according to claim 1, wherein the extrusion barrel, the extrusion cavities, the extrusion head, the pressure applying head, the extrusion ejector rods, the fiber core extrusion pieces and the extrusion dies are all subjected to ultrasonic cleaning and alcohol wiping before use, and the fiber core glass ingot and the cladding glass ingot are both washed by alcohol and deionized water before use.
3. The method of claim 1, wherein steps 7-11 are performed in a vacuum environment of a vacuum chamber.
4. The extrusion method for preparing a high polarization maintaining microstructure optical fiber preform according to claim 3, wherein the vacuum environment of the vacuum chamber is obtained by processing as follows: vacuumizing the vacuum chamber by using a vacuum pump, so that the vacuum degree in the vacuum chamber is lower than 10-2And when Pa is needed, supplementing inert gas into the vacuum cavity to enable the air pressure in the vacuum cavity to be the same as the external atmospheric pressure.
5. The extrusion preparation method of the high polarization maintaining microstructure optical fiber preform rod as claimed in any one of claims 1 to 4, wherein the shapes of the core extrusion holes of the extrusion dies in the extrusion die set are not identical.
6. The extrusion method of claim 5, wherein each extrusion chamber is detachably fastened to the bottom of the extrusion head.
7. The extrusion method for preparing a high polarization maintaining microstructure optical fiber preform according to any one of claims 1 to 4, wherein the predetermined time in step 11 is 4 to 12 hours.
8. The extrusion method for preparing the high polarization maintaining microstructure optical fiber preform according to any one of claims 1 to 4, wherein each of the core glass ingot and the cladding glass ingot is a chalcogenide glass ingot.
9. The extrusion method of claim 8, wherein the core glass ingot is Ge9As23Se68The cladding glass ingot is Ge10As22Se68。
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