CN114560628B - Preparation method of local three-dimensional microstructure optical fiber - Google Patents
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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
- C03B37/01268—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 casting
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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
- C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
- C03B37/025—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from reheated softened tubes, rods, fibres or filaments, e.g. drawing fibres from preforms
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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
- C03B37/10—Non-chemical treatment
- C03B37/14—Re-forming fibres or filaments, i.e. changing their shape
- C03B37/15—Re-forming fibres or filaments, i.e. changing their shape with heat application, e.g. for making optical fibres
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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
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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
- C03C13/045—Silica-containing oxide glass compositions
- C03C13/046—Multicomponent glass compositions
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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
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/66—Chemical treatment, e.g. leaching, acid or alkali treatment
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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
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/66—Chemical treatment, e.g. leaching, acid or alkali treatment
- C03C25/68—Chemical treatment, e.g. leaching, acid or alkali treatment by etching
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/24—Coupling light guides
- G02B6/255—Splicing of light guides, e.g. by fusion or bonding
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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Abstract
The embodiment of the invention discloses a preparation method of a local three-dimensional microstructure optical fiber, which comprises the following steps: s1, preparing a sodium borosilicate glass rod; s2, preparing three-dimensional glass fibers; s3, preparing three-dimensional quartz glass fibers; s4, preparing the local three-dimensional microstructure optical fiber. According to the invention, the operation is simple, the three-dimensional microstructure optical fiber with various forms can be obtained, and the production cost is remarkably reduced.
Description
Technical Field
The invention relates to the technical field of optical fibers with three-dimensional structures, in particular to a preparation method of a local three-dimensional microstructure optical fiber.
Background
The glass fiber is a fiber-shaped glass which is colorless, transparent and glossy, has high tensile strength, high elastic coefficient, good chemical resistance and heat resistance and good light transmittance, and is easy to process into different products such as strands, bundles, felts, fabrics and the like; the glass fiber has low price and wide application: glass ropes, glass cloth, insulating materials, glass fiber composite materials, glass wool, fiber endoscopes, optical fibers and the like. Although glass fibers have many advantages as described above, the following technical problems remain in the process of preparing glass fibers into three-dimensional structured optical fibers:
the preparation process is complicated, so that the production cost is high, and the popularization and the use of the three-dimensional structure optical fiber in a plurality of application fields are seriously influenced.
In view of the foregoing, there is a need for a method for preparing a local three-dimensional microstructured optical fiber to solve the above-mentioned problems.
Disclosure of Invention
The embodiment of the invention provides a preparation method of a local three-dimensional microstructure optical fiber, which is simple to operate and capable of obtaining three-dimensional microstructure optical fibers in various forms, and remarkably reduces production cost.
In order to solve the technical problems, the embodiment of the invention discloses the following technical scheme:
the preparation method of the local three-dimensional microstructure optical fiber comprises the following steps:
s1, preparing a sodium borosilicate glass rod: raw material Na 2 CO 3 、H 3 BO 3 、SiO 2 Uniformly mixing according to a designed proportion, pouring into a crucible, melting for 3 hours at 1300-1500 ℃ to prepare sodium borosilicate glass, and then obtaining a sodium borosilicate glass rod through casting treatment;
s2, preparing three-dimensional glass fibers: stacking and stretching the sodium borosilicate glass rods prepared in the step S1 to obtain three-dimensional glass fibers;
s3, preparing three-dimensional quartz glass fibers: carrying out surface flushing on the three-dimensional glass fiber prepared in the step S2 by deionized water, and then placing the flushed three-dimensional glass fiber in a tube furnace for heat treatment; then, soaking the three-dimensional glass fiber subjected to heat treatment in an ammonium bifluoride solution for pretreatment; finally, placing the three-dimensional glass fiber after pretreatment into an oil bath pot with the temperature of 80-90 ℃ for acid treatment, and obtaining the three-dimensional quartz glass fiber;
s4, preparing a local three-dimensional microstructure optical fiber: and (3) welding the three-dimensional quartz glass fiber obtained after the acid treatment prepared in the step (S3) with the one-dimensional optical fiber at a set temperature to obtain the local three-dimensional microstructure optical fiber.
In addition to one or more features and/or steps disclosed above, or alternatively, the three-dimensional glass fibers in step S2 are stacked as a three-dimensional solid structure or a three-dimensional hollow structure.
In addition to one or more of the features and/or steps disclosed above, or alternatively, the time of the heat treatment in step S3 is 12-36 hours, the temperature is controlled to 520-580 ℃, and the temperature rising rate is controlled to 10-15 ℃/min.
In addition to one or more of the features and/or steps disclosed above, or as an alternative, the concentration of ammonium bifluoride solution used for the pretreatment in step S3 is 1-2mol/L, the pretreatment time not exceeding 40S.
In addition to one or more of the features and/or steps disclosed above, or as an alternative, the solution used for the acid treatment in step S3 is HCL at a concentration of 0.25 to 0.5mol/L for a period of 12 to 36 hours.
In addition to, or in lieu of, one or more of the features and/or steps disclosed above, the acid treatment solution in step S3 contains a buffer, which is NH 4 Cl and Na 2 SO 3 Wherein, HCl, NH 4 Cl and Na 2 SO 3 The three materials are mixed in a volume ratio of 1:1:1 to form the mixed acid liquid.
In addition to one or more of the features and/or steps disclosed above, or as an alternative, in step S4, the temperature of the fusion process is controlled to be in the range of 1000-1200 ℃ in such a way that at least one segment of three-dimensional quartz glass fibers is fused to one-dimensional fibers.
In addition to or instead of one or more of the features and/or steps disclosed above, in step S1, the raw materials are designed in proportions by mass:
GeNO 3 5～15wt％；
Na 2 CO 3 51～61wt％；
H 3 BO 3 21～31wt％；
SiO 2 3～13wt％。
one of the above technical solutions has the following advantages or beneficial effects: the preparation process is simple to operate and the three-dimensional glass fiber obtained by the preparation is various in forms due to the fact that the three-dimensional glass fiber is prepared through stacking and stretching.
The other technical scheme has the following advantages or beneficial effects: the fused optical fiber with the local three-dimensional microstructure has the advantages of three-dimensional quartz glass fiber structure, such as low refractive index, low numerical aperture, stable mode and easy bending, and also compensates the limitations of the traditional one-dimensional optical fiber in application, such as high refractive index, unstable mode and difficult bending.
Drawings
The technical solution and other advantageous effects of the present invention will be made apparent by the following detailed description of the specific embodiments of the present invention with reference to the accompanying drawings.
FIG. 1 is a flow chart of a method for preparing a local area three-dimensional microstructured optical fiber according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a local three-dimensional microstructured optical fiber according to embodiment 1 of the present invention;
FIG. 3 is a schematic view of a local three-dimensional microstructured optical fiber according to embodiment 2 of the present invention;
FIG. 4 is a schematic view of a local three-dimensional microstructured optical fiber according to embodiment 3 of the present invention;
FIG. 5 is a schematic view of a local three-dimensional microstructured optical fiber according to embodiment 4 of the present invention;
reference numerals in the drawings are respectively:
11. solid sodium borosilicate glass rods; 12. Hollow quartz sodium borosilicate glass rod;
14. sodium borosilicate glass sleeve; 21. Solid sodium borosilicate glass rods;
22. solid quartz sodium borosilicate glass rod; 24. Sodium borosilicate glass sleeve;
31. hollow quartz sodium borosilicate glass rod; 32. Solid sodium borosilicate glass rods;
34. sodium borosilicate glass sleeve; 41. Solid quartz sodium borosilicate glass rod;
42. solid sodium borosilicate glass rods; 44. Sodium borosilicate glass sleeve.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more of the described features. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
Example 1
Referring to fig. 1 and fig. 2, fig. 1 is a flowchart of a preparation method of a local three-dimensional microstructure optical fiber according to an embodiment of the present invention; fig. 2 is a schematic diagram of a local three-dimensional microstructured optical fiber according to the present embodiment. The method provided by the embodiment aims to reduce the process complexity of preparing the glass fiber into the three-dimensional structure optical fiber and enable the three-dimensional microstructure optical fiber obtained by preparation to be various in form. The preparation method of the local three-dimensional microstructure optical fiber provided by the embodiment comprises the following steps:
s1, preparing a sodium borosilicate glass rod: 10 parts by weight of GeNO of high-purity raw material 3 56 parts by weight of Na 2 CO 3 26 parts by weight of H 3 BO 3 8 parts by weight of SiO 2 Uniformly mixing, pouring into a platinum crucible, melting for 3 hours at the high temperature of 1300 ℃ to prepare sodium borosilicate glass, and then casting to obtain a sodium borosilicate glass rod with the diameter of 5 mm;
s2, preparing three-dimensional glass fibers: stacking and stretching the sodium borosilicate glass rods prepared in the step S1 to obtain three-dimensional glass fibers; specifically, in the non-limiting embodiment shown in FIG. 2, 7 hollow quartz sodium borosilicate glass rods 12 of 5mm diameter are placed in a 5cm long sodium borosilicate glass sleeve 14, stacked in shape and drawn on a drawing machine into three-dimensional sodium borosilicate glass fibers 15 of 125 μm diameter;
s3, preparing three-dimensional quartz glass fibers: carrying out surface flushing on the sodium borosilicate glass fiber 15 with the diameter of 125 mu m prepared in the step S2 by deionized water, and then placing the flushed three-dimensional sodium borosilicate glass fiber 15 in a tube furnace for heat treatment for a period of time, specifically, carrying out phase separation at 520 ℃ for 12 hours at a heating rate of 8 ℃/min; subsequently, the three-dimensional sodium borosilicate glass fiber 15 was immersed in ammonium bifluoride at a concentration of 1mol/L for 30 seconds; finally, repeatedly washing the surface with alcohol and deionized water, drying, and then placing the three-dimensional sodium borosilicate glass fiber 15 in 0.25mol/L HCl for acid treatment, wherein the temperature of an oil bath pot is 90 ℃, the acid treatment time is 12h, and the buffer used is NH 4 Cl and Na 2 SO 3 Wherein HCl, NH 4 Cl and Na 2 SiO 3 Na 2 SO 3 The volume ratio of the three is 1:1:1, mixed acid liquid is formed, and the three-dimensional quartz glass fiber with the length of 5cm is obtained after drying;
s4, preparing a local three-dimensional microstructure optical fiber: in the fusion process shown in FIG. 2, a 5mm diameter rod of sodium borosilicate glass was drawn into two solid sodium borosilicate glass fibers 11 of 125 μm diameter and placed on both sides of a 125 μm diameter three-dimensional hollow silica glass fiber, and then the two solid sodium borosilicate glass fibers 11 were fused with the three-dimensional hollow silica glass fiber at 1200 ℃.
Hereinafter and throughout the specification, the term "one-dimensional optical fiber" is understood to mean a fiber drawn from a single glass rod, and the term "three-dimensional optical fiber" is understood to mean an optical fiber drawn from three-dimensionally stacked glass rods.
Hereinafter and throughout the specification, the term "high purity" should be understood as that the purity of the main component of each raw material should reach 99.5% and above.
Example 2
Referring to fig. 1 and 3, fig. 1 is a flowchart of a preparation method of a local three-dimensional microstructure optical fiber according to an embodiment of the present invention; fig. 3 is a schematic diagram of a local three-dimensional microstructured optical fiber according to the present embodiment. The method provided by the embodiment aims to reduce the process complexity of preparing the glass fiber into the three-dimensional structure optical fiber and enable the three-dimensional microstructure optical fiber obtained by preparation to be various in form. The preparation method of the local three-dimensional microstructure optical fiber provided by the embodiment comprises the following steps:
s1, preparing a sodium borosilicate glass rod: 5 parts by weight of high-purity raw material GeNO 3 61 parts by weight of Na 2 CO 3 31 parts by weight of H 3 BO 3 3 parts by weight of SiO 2 Uniformly mixing, pouring into a platinum crucible, melting for 3 hours at the high temperature of 1300 ℃ to prepare sodium borosilicate glass, and then casting to obtain a sodium borosilicate glass rod with the diameter of 5 mm;
s2, preparing three-dimensional glass fibers: stacking and stretching the sodium borosilicate glass rods prepared in the step S1 to obtain three-dimensional glass fibers; specifically, in the non-limiting embodiment shown in FIG. 3, 7 hollow sodium borosilicate glass rods 22 of 5mm diameter are placed in a 5cm long sodium borosilicate glass sleeve 24, and after stacking the shapes, drawn on a wire drawing machine into three-dimensional sodium borosilicate glass fibers 25 of 125 μm diameter;
s3, preparing three-dimensional quartz glass fibers: carrying out surface flushing on the three-dimensional sodium borosilicate glass fiber 25 with the diameter of 125 mu m prepared in the step S2 by deionized water, and then placing the flushed three-dimensional sodium borosilicate glass fiber 25 in a tube furnace for heat treatment for a period of time, specifically, carrying out phase separation for 12 hours at 540 ℃ at a heating rate of 10 ℃/min; subsequently, the three-dimensional sodium borosilicate glass fiber 25 was immersed in ammonium bifluoride at a concentration of 1mol/L for 30 seconds; finally, repeatedly washing the surface with alcohol and deionized water, drying, and then placing the three-dimensional sodium borosilicate glass fiber 25 in 0.5mol/L HCl for acid treatment, wherein the temperature of the oil bath pot is 90 ℃, the acid treatment time is 14h, and the buffer used is NH 4 Cl and Na 2 SO 3 Wherein HCl, NH 4 Cl and Na 2 SO 3 The volume ratio of the three is 1:1:1, mixed acid liquid is formed, and the three-dimensional quartz glass fiber with the length of 5cm is obtained after drying;
s4, preparing a local three-dimensional microstructure optical fiber: in the fusion process shown in FIG. 3, a 5mm diameter rod of sodium borosilicate glass was drawn into two solid sodium borosilicate glass fibers 21 of 5cm diameter and 125 μm diameter, the two solid sodium borosilicate glass fibers 21 of 125 μm diameter were placed on both sides of the 125 μm diameter three-dimensional solid sodium borosilicate glass fibers, and then the two solid sodium borosilicate glass fibers 21 and the three-dimensional solid sodium borosilicate glass fibers were fused at 1200 ℃.
Example 3
Referring to fig. 1 and fig. 4, fig. 1 is a flowchart of a preparation method of a local three-dimensional microstructure optical fiber according to an embodiment of the present invention; fig. 4 is a schematic diagram of a local three-dimensional microstructured optical fiber according to the present embodiment. The method provided by the embodiment aims to reduce the process complexity of preparing the glass fiber into the three-dimensional structure optical fiber and enable the three-dimensional microstructure optical fiber obtained by preparation to be various in form. The preparation method of the local three-dimensional microstructure optical fiber provided by the embodiment comprises the following steps:
s1, preparing a sodium borosilicate glass rod: 15 parts by weight of GeNO of high-purity raw material 3 51 parts by weight of Na 2 CO 3 21 parts by weight of H 3 BO 3 13 parts by weight of SiO 2 Uniformly mixing, pouring into a platinum crucible, melting for 3 hours at the high temperature of 1300 ℃ to prepare sodium borosilicate glass, and then casting to obtain a sodium borosilicate glass rod with the diameter of 5 mm;
s2, preparing three-dimensional glass fibers: stacking and stretching the sodium borosilicate glass rods prepared in the step S1 to obtain three-dimensional glass fibers; specifically, in the non-limiting embodiment shown in FIG. 4, 7 hollow sodium borosilicate glass rods 32 of 5mm diameter are placed in a 5cm long sodium borosilicate glass sleeve 34, and after stacking the shapes, drawn on a wire drawing machine into three-dimensional sodium borosilicate glass fibers 35 of 125 μm diameter;
s3, preparing three-dimensional quartz glass fibers: surface-washing the three-dimensional sodium borosilicate glass fiber 35 having a diameter of 125 μm prepared in step S2 with deionized water, and then heat-treating the washed three-dimensional sodium borosilicate glass fiber 35 in a tube furnace for a period of time, specifically, at a heating rate of 8 ℃/min at 520 ℃ for a period of timePhase 12h; subsequently, the three-dimensional sodium borosilicate glass fiber 35 was immersed in ammonium bifluoride at a concentration of 1mol/L for 30 seconds; finally, repeatedly washing the surface with alcohol and deionized water, drying, and then placing the three-dimensional sodium borosilicate glass fiber 35 in 0.25mol/L HCl for acid treatment, wherein the temperature of the oil bath pot is 90 ℃, the acid treatment time is 12h, and the buffer used is NH 4 Cl and Na 2 SO 3 Wherein HCl, NH 4 Cl and Na 2 SO 3 The volume ratio of the three is 1:1:1, mixed acid liquid is formed, and the three-dimensional quartz glass fiber with the length of 5cm is obtained after drying;
s4, preparing a local three-dimensional microstructure optical fiber: in the fusion process shown in FIG. 4, a 5mm diameter rod of sodium borosilicate glass was drawn into a 5cm diameter solid sodium borosilicate glass fiber 32 having a diameter of 125 μm, two 125 μm diameter three-dimensional hollow silica glass fibers were placed on both sides of the 125 μm diameter solid sodium borosilicate glass fiber 35, and then the two three-dimensional hollow silica glass fibers were fused with the solid sodium borosilicate glass fiber 35 at 1200 ℃.
Example 4
Referring to fig. 1 and 3, fig. 1 is a flowchart of a preparation method of a local three-dimensional microstructure optical fiber according to an embodiment of the present invention; fig. 3 is a schematic diagram of a local three-dimensional microstructured optical fiber according to the present embodiment. The method provided by the embodiment aims to reduce the process complexity of preparing the glass fiber into the three-dimensional structure optical fiber and enable the three-dimensional microstructure optical fiber obtained by preparation to be various in form. The preparation method of the local three-dimensional microstructure optical fiber provided by the embodiment comprises the following steps:
s1, preparing a sodium borosilicate glass rod: 8 parts by weight of high-purity raw material GeNO 3 58 parts by weight of Na 2 CO 3 23 parts by weight of H 3 BO 3 11 parts by weight of SiO 2 Uniformly mixing, pouring into a platinum crucible, melting for 3 hours at the high temperature of 1300 ℃ to prepare sodium borosilicate glass, and then casting to obtain a sodium borosilicate glass rod with the diameter of 5 mm;
s2, preparing three-dimensional glass fibers: stacking and stretching the sodium borosilicate glass rods prepared in the step S1 to obtain three-dimensional glass fibers; specifically, in the non-limiting embodiment shown in FIG. 5, 7 solid sodium borosilicate glass rods 42 of 5mm diameter are placed in a 5cm long sodium borosilicate glass sleeve 44, and after stacking the shapes, drawn on a wire drawing machine into three-dimensional sodium borosilicate glass fibers 45 of 125 μm diameter;
s3, preparing three-dimensional quartz glass fibers: carrying out surface flushing on the three-dimensional sodium borosilicate glass fiber 45 with the diameter of 125 mu m prepared in the step S2 by deionized water, and then carrying out heat treatment on the flushed three-dimensional sodium borosilicate glass fiber 45 in a tube furnace for a period of time, specifically, carrying out phase separation at 520 ℃ for 12 hours at a heating rate of 8 ℃/min; subsequently, the three-dimensional sodium borosilicate glass fiber 45 was immersed in ammonium bifluoride at a concentration of 1mol/L for 30 seconds; finally, repeatedly washing the surface with alcohol and deionized water, drying, and then placing the three-dimensional sodium borosilicate glass fiber 45 in 0.25mol/L HCl for acid treatment, wherein the temperature of an oil bath pot is 90 ℃, the acid treatment time is 14h, and the buffer used is NH 4 Cl and Na 2 SO 3 Wherein HCl, NH 4 Cl and Na 2 SO 3 The volume ratio of the three is 1:1:1, mixed acid liquid is formed, and the three-dimensional quartz glass fiber with the length of 5cm is obtained after drying;
s4, preparing a local three-dimensional microstructure optical fiber: in the fusion process shown in FIG. 3, a 5mm diameter rod of sodium borosilicate glass was drawn into a 5cm diameter solid sodium borosilicate glass fiber with a diameter of 125 μm, two 125 μm diameter three-dimensional solid quartz glass fibers were placed on both sides of the 125 μm diameter solid sodium borosilicate glass fiber, and then, two 125 μm diameter three-dimensional solid quartz glass fibers were fused with the solid sodium borosilicate glass fiber at 1200 ℃.
The above describes in detail the preparation method of a local three-dimensional microstructure optical fiber provided by the embodiment of the present invention, and specific examples are applied to illustrate the principle and implementation of the present invention, and the description of the above examples is only used to help understand the technical scheme and core idea of the present invention; those of ordinary skill in the art will appreciate that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (5)
1. The preparation method of the local three-dimensional microstructure optical fiber is characterized by comprising the following steps of:
s1, preparing a sodium borosilicate glass rod: geNO as raw material 3 、Na 2 CO 3 、H 3 BO 3 、SiO 2 Uniformly mixing according to a designed proportion, pouring into a crucible, melting for 3 hours at 1300-1500 ℃ to prepare sodium borosilicate glass, and then obtaining a sodium borosilicate glass rod through casting treatment;
s2, preparing three-dimensional glass fibers: stacking and stretching the sodium borosilicate glass rods prepared in the step S1 to obtain three-dimensional glass fibers;
s3, preparing three-dimensional quartz glass fibers: carrying out surface flushing on the three-dimensional glass fiber prepared in the step S2 by deionized water, and then placing the flushed three-dimensional glass fiber in a tube furnace for heat treatment; then, soaking the three-dimensional glass fiber subjected to heat treatment in an ammonium bifluoride solution for pretreatment; finally, placing the three-dimensional glass fiber after pretreatment into an oil bath pot with the temperature of 80-90 ℃ for acid treatment, and obtaining the three-dimensional quartz glass fiber;
s4, preparing a local three-dimensional microstructure optical fiber: instantly welding the three-dimensional quartz glass fiber obtained after the acid treatment prepared in the step S3 with the one-dimensional fiber at the set temperature of 1000-1200 ℃ in a way that at least one section of three-dimensional quartz glass fiber is welded on the one-dimensional fiber, so as to obtain the local three-dimensional microstructure fiber;
wherein the concentration of the ammonium bifluoride solution used for pretreatment in the step S3 is 1-2mol/L, and the pretreatment time is not more than 40S;
in the step S1, the design proportion of the raw materials is as follows:
2. the method of manufacturing a localized three-dimensional microstructured optical fiber of claim 1, wherein the three-dimensional glass fibers of step S2 are stacked in a three-dimensional solid structure or a three-dimensional hollow structure.
3. The method for preparing a localized three-dimensional microstructured optical fiber according to claim 1, wherein the time of the heat treatment in step S3 is 12-36 hours, the temperature is controlled at 520-580 ℃, and the heating rate is controlled at 10-15 ℃/min.
4. The method for preparing a localized three-dimensional microstructured optical fiber according to claim 1, wherein the solution used for the acid treatment in step S3 is HCl with a concentration of 0.25 to 0.5mol/L, and the acid treatment time is 12 to 36 hours.
5. The method of preparing a localized three-dimensional microstructured optical fiber of claim 4 wherein the acid treatment solution of step S3 comprises a buffer agent, the buffer agent being NH 4 Cl and Na 2 SO 3 Wherein, HCl, NH 4 Cl and Na 2 SO 3 The three materials are mixed in a volume ratio of 1:1:1 to form the mixed acid liquid.
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| CN202210276106.9A CN114560628B (en) | 2022-03-21 | 2022-03-21 | Preparation method of local three-dimensional microstructure optical fiber |
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| CN202210276106.9A CN114560628B (en) | 2022-03-21 | 2022-03-21 | Preparation method of local three-dimensional microstructure optical fiber |
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| CN114560628A CN114560628A (en) | 2022-05-31 |
| CN114560628B true CN114560628B (en) | 2023-05-26 |
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| CN214539244U (en) * | 2020-11-19 | 2021-10-29 | 重庆三峡学院 | Temperature compensated SPR sensor with large measurement range |
| CN114034665A (en) * | 2021-12-02 | 2022-02-11 | 天津工业大学 | Reflection micro-flow sensing device based on single-hole microstructure optical fiber |
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| FR2427621A1 (en) * | 1978-05-30 | 1979-12-28 | Thomson Csf | LOW ATTENUATION OPTICAL FIBER MANUFACTURING PROCESS, AND OPTICAL FIBER OBTAINED BY THIS PROCESS |
| JP2002293562A (en) * | 2001-03-29 | 2002-10-09 | Sumitomo Electric Ind Ltd | Method for producing optical fiber |
| US6652163B2 (en) * | 2001-10-31 | 2003-11-25 | Corning Incorporated | Splice joint and process for joining a microstructured optical fiber and a conventional optical fiber |
| CN1278969C (en) * | 2004-12-13 | 2006-10-11 | 天津大学 | Precasting method of optical fibre with microstructure |
| CN101710193A (en) * | 2009-11-27 | 2010-05-19 | 电子科技大学 | Method for manufacturing microstructure fiber |
| CN103936276B (en) * | 2014-03-31 | 2016-06-29 | 陈抗抗 | A kind of preparation method of microstructured optical fibers |
| GB201911183D0 (en) * | 2019-08-05 | 2019-09-18 | Lumenisity Ltd | Optical fibre splicing method |
| CN110515159B (en) * | 2019-08-15 | 2020-06-02 | 华中科技大学 | LP based on fiber end face microstructure01-LPmnAll-fiber mode converter and preparation method thereof |
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| CN214539244U (en) * | 2020-11-19 | 2021-10-29 | 重庆三峡学院 | Temperature compensated SPR sensor with large measurement range |
| CN114034665A (en) * | 2021-12-02 | 2022-02-11 | 天津工业大学 | Reflection micro-flow sensing device based on single-hole microstructure optical fiber |
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