CN111087182A - Chemical corrosion preparation method of chalcogenide glass tapered optical fiber - Google Patents
Chemical corrosion preparation method of chalcogenide glass tapered optical fiber Download PDFInfo
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- CN111087182A CN111087182A CN202010024511.2A CN202010024511A CN111087182A CN 111087182 A CN111087182 A CN 111087182A CN 202010024511 A CN202010024511 A CN 202010024511A CN 111087182 A CN111087182 A CN 111087182A
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- 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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Abstract
The invention discloses a chemical corrosion preparation method of a chalcogenide glass tapered optical fiber, which comprises the steps of preparing a sodium hydroxide solution, removing a chalcogenide glass optical fiber coating layer, preparing a corrosion device, fixing and protecting a chalcogenide glass bare optical fiber, chemically corroding the chalcogenide glass bare optical fiber and the like. The method has simple process, strong operability and lower cost, and can prepare a smoother tapered optical fiber surface by controlling process parameters such as the mass concentration of a reasonable sodium hydroxide solution, the chemical corrosion time and the like, the outer diameter of the cladding of the prepared chalcogenide glass optical fiber is controllable and adjustable, the outer diameter of the fiber core of the chalcogenide glass optical fiber is kept unchanged, and the loss is lower; the optical fiber sensor manufactured by the chalcogenide glass tapered optical fiber prepared by the method is very sensitive to bending, temperature, strain, refractive index and the like, has low cost, is simple to manufacture, has good controllability and high efficiency, can realize mass production, and has good application prospect in the field of optical fiber communication and sensing.
Description
Technical Field
The invention relates to a preparation method of a chalcogenide glass tapered optical fiber, in particular to a chemical corrosion preparation method of the chalcogenide glass tapered optical fiber.
Background
Tapered fibers are fibers that are tapered by physical or chemical means. According to the difference of the diameters of the tapered optical fibers, optical fields with different percentages are transmitted outside the optical fibers in the form of evanescent waves, and the evanescent waves can sense the change of certain parameters of the external environment, so that the sensitivity and the response speed of the optical fiber sensor are remarkably improved, and the optical fiber sensor has more advantages in sensing application.
The current method for preparing tapered optical fibers is mainly a fusion tapering method. The tapered optical fiber manufactured by the fusion-draw method is characterized in that the diameters of the cladding and the core of the optical fiber are tapered along the axial direction of the optical fiber, and the ratio of the diameters of the cladding and the core is generally considered to be constant in the whole tapered region. The method has the advantages of simple process, strong operability, good repeatability and high accuracy, but the diameters of the core and the cladding of the optical fiber are reduced simultaneously in the fusion tapering process, namely the diameter of the core is reduced while the cladding of the optical fiber is tapered, which is not allowed in some experiments or applications which want to keep the diameter of the core unchanged. Meanwhile, the loss of the melting tapering method is high, and particularly for chalcogenide glass optical fibers used in infrared bands, the problems of low mechanical strength, easy breakage, easy oxidation during heating and the like exist, so that the preparation efficiency and the quality of the chalcogenide glass tapered optical fibers are severely restricted.
Disclosure of Invention
The invention aims to solve the technical problem of providing a chemical corrosion preparation method of a chalcogenide glass tapered optical fiber, which has the advantages of simple process, strong operability, low loss and low cost, aiming at the defects of the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows: a chemical corrosion preparation method of chalcogenide glass tapered optical fiber comprises the following steps:
(1) preparing sodium hydroxide solution
Preparing a proper amount of sodium hydroxide solution with a certain concentration, and cooling to room temperature for later use;
(2) removal of chalcogenide glass optical fiber coating
Preparing a chalcogenide glass optical fiber, wherein the structure of the chalcogenide glass optical fiber comprises a fiber core, a cladding and a coating layer, the fiber core and the cladding are both made of chalcogenide glass, and the coating layer is a high polymer layer;
intercepting a section of chalcogenide glass optical fiber, soaking the chalcogenide glass optical fiber in dimethylacetamide, removing a coating layer on the surface of the chalcogenide glass optical fiber to obtain a bare fiber, soaking the bare fiber in alcohol, washing off the dimethylacetamide remaining on the surface of the bare fiber, taking out the bare fiber, and wiping and cleaning the surface of the bare fiber for later use;
(3) preparation of etching apparatus
Preparing a corrosion device, wherein the corrosion device comprises a container, an alkali liquor supply unit and an alkali liquor collection unit, a liquid guide channel is arranged in the container, a first concave positioning groove, a second concave positioning groove and a groove which penetrate through the container in the length direction are arranged at the upper part of the container, the groove is communicated with the liquid guide channel up and down, the width of the groove is larger than the outer diameter of the liquid guide channel, the length of the groove is matched with the length of a conical area of a conical optical fiber to be prepared, the first positioning groove and the second positioning groove are respectively arranged at two sides of the groove and are respectively communicated with the groove horizontally, the axis of the first positioning groove and the axis of the second positioning groove are on the same straight line, and the connecting line of the axis of the first positioning groove and the axis of the second positioning groove transversely penetrates through the groove, the widths of the first positioning groove and the second positioning groove are respectively matched with the outer diameter of the bare optical fiber, the liquid outlet of the alkali liquor supply unit is communicated with one end of the liquid guide channel, and the other end of the liquid guide channel is communicated with the liquid inlet of the alkali liquor collection unit; the alkali liquor supply unit is used for continuously introducing a sodium hydroxide solution into the liquid guide channel, and the alkali liquor collection unit is used for collecting the sodium hydroxide solution discharged from the liquid guide channel; a CCD camera connected with a computer is suspended above the container, and a lens of the CCD camera faces downwards and is opposite to the groove;
(4) fixing and protecting chalcogenide glass bare optical fiber
Fixing the bare optical fiber obtained in the step (2) on an optical fiber clamp, tightly pressing two ends of the bare optical fiber through the optical fiber clamp, placing a three-dimensional optical adjusting frame below the bare optical fiber, placing the container on the top of the three-dimensional optical adjusting frame, adjusting the distance between the optical fiber clamp and the container through the three-dimensional optical adjusting frame, respectively embedding two sides of the bare optical fiber into the first positioning groove and the second positioning groove, and enabling the middle part of the bare optical fiber to be positioned in the groove;
(5) chemical corrosion of chalcogenide glass bare fiber
Pouring the sodium hydroxide solution prepared in the step (1) into the alkali liquor supply unit, starting the alkali liquor supply unit, continuously introducing the sodium hydroxide solution into the liquid guide channel, keeping the liquid level of the sodium hydroxide solution in the groove above the upper surface of the bare fiber, the surface of the middle part of the bare fiber is chemically corroded by the sodium hydroxide solution in the groove, the outer diameter of the bare fiber is observed in real time by a CCD camera, when the outer diameter of the bare fiber reaches a predetermined value, the alkali supply unit is closed, the container is removed, a glass slide is placed on the top of the three-dimensional optical adjusting frame, the glass slide is slowly lifted through the three-dimensional optical adjusting frame, so that the upper surface of the glass slide just contacts with the lower surface of the bare fiber, and fixing two ends of the bare fiber on a glass slide, finally cleaning the surface of the bare fiber by using deionized water and alcohol, and drying to obtain the chalcogenide glass tapered fiber.
Preferably, the mass concentration of the sodium hydroxide solution prepared in the step (1) is 2-10%, and the corrosion time of the surface of the middle part of the bare fiber in the step (5) is 2-5 min.
Preferably, in the step (2), the chalcogenide glass optical fiber is As2S3、As2Se3Ge-As-Se or Ge-As-S chalcogenide glass fibers.
Preferably, the outer diameter of the cladding in the step (2) is 150 to 300 μm, and the outer diameter of the core is 10 to 100 μm.
Preferably, the environmental temperature for the chemical etching in the step (5) is 25 to 50 ℃.
Compared with the prior art, the invention has the following advantages:
1. the chemical corrosion preparation method of the chalcogenide glass tapered optical fiber disclosed by the invention has the advantages of simple process, strong operability and lower cost, the smoother tapered optical fiber surface can be prepared by controlling process parameters such as reasonable mass concentration of sodium hydroxide solution, chemical corrosion time and the like, the outer diameter of the cladding of the prepared chalcogenide glass optical fiber is controllable and adjustable, the outer diameter of the fiber core of the chalcogenide glass optical fiber is kept unchanged, and the loss is lower;
2. the optical fiber sensor manufactured by the chalcogenide glass tapered optical fiber prepared by the method is very sensitive to bending, temperature, strain, refractive index and the like, has low cost, is simple to manufacture, has good controllability and high efficiency, can realize mass production, and has good application prospect in the field of optical fiber communication and sensing.
Drawings
FIG. 1 is a top view of the container in the example;
FIG. 2 is a left side view of the container in the embodiment;
FIG. 3 shows multimode As obtained in example 12S3A cross-sectional photograph of the tapered region of the chalcogenide glass tapered fiber;
FIG. 4 shows multimode As obtained in example 12S3A photograph of the lengthwise appearance of the tapered region of the chalcogenide glass tapered fiber;
FIG. 5 shows multimode As in example 12S3Corrosion time-cladding diameter curve of chalcogenide glass tapered fiber;
FIG. 6 shows the multi-mode Ge obtained in example 210As24S66A cross-sectional photograph of the tapered region of the chalcogenide glass tapered fiber;
FIG. 7 shows the multimode Ge obtained in example 210As24S66A photograph of the lengthwise appearance of the tapered region of the chalcogenide glass tapered fiber;
FIG. 8 shows the multi-mode Ge of example 210As24S66Sodium hydroxide solution concentration-cladding diameter curve for chalcogenide glass tapered fibers.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
Example 1: in multiple modes of As2S3The chalcogenide glass tapered optical fiber is taken As an example, and the multimode As is prepared by adopting the chemical corrosion preparation method of the invention2S3The chalcogenide glass tapered optical fiber comprises the following steps:
(1) preparing sodium hydroxide solution
Preparing a proper amount of sodium hydroxide solution with the mass concentration of 4%, and cooling to room temperature for later use;
(2) removal of chalcogenide glass optical fiber coating
Preparing a multimode As2S3Chalcogenide glass optical fiber, the multimode As2S3The chalcogenide glass optical fiber comprises a core with an outer diameter of 61 μm, a cladding with an outer diameter of 277 μm, and a coating layer2S3The coating layer is a high polymer layer;
the optical fiber cutter cuts a section of multimode As with the length of 10cm2S3The chalcogenide glass optical fiber is immersed in dimethylacetamide (with purity of 99% or more) to remove multimode As2S3Coating the surface of the chalcogenide glass optical fiber to obtain a bare fiber, soaking the bare fiber in alcohol (purchased from outsourcing, the purity of which is more than 99.7%) for 30s, washing off residual dimethylacetamide on the surface of the bare fiber, taking out the bare fiber, and wiping and cleaning the surface of the bare fiber for later use;
(3) preparation of etching apparatus
Preparing an etching device, as shown in figure 1, the etching device comprises a container 1, an alkali liquor supply unit and an alkali liquor collection unit, as shown in figures 1-2, a liquid guide channel is arranged in the container 1, a first concave positioning groove 11, a second concave positioning groove 12 and a groove 13 which penetrate through the container 1 in the length direction are arranged at the upper part of the container 1, the groove 13 is communicated with the liquid guide channel up and down, the width of the groove 13 is larger than the outer diameter of the liquid guide channel, the length of the groove 13 is matched with the length of a conical area of a conical optical fiber to be prepared, the first positioning groove 11 and the second positioning groove 12 are respectively arranged at two sides of the groove 13 and are respectively communicated with the groove 13 horizontally, the axial line of the first positioning groove 11 and the axial line of the second positioning groove 12 are on the same straight line, the connecting line of the axial line of the first positioning groove 11 and the axial line of the second positioning groove 12 traverses the groove 13, the widths of the first positioning groove 11 and the second positioning groove 12, the liquid outlet of the alkali liquor supply unit is communicated with one end of the liquid guide channel, and the other end of the liquid guide channel is communicated with the liquid inlet of the alkali liquor collection unit; the alkali liquor supply unit is used for continuously introducing a sodium hydroxide solution into the liquid guide channel, and the alkali liquor collection unit is used for collecting the sodium hydroxide solution discharged from the liquid guide channel; a CCD camera connected with a computer is suspended above the container 1, and a lens of the CCD camera faces downwards and is opposite to the groove 13;
in the embodiment, the length of the container 1 is 10-15 cm, the width is 2-5 cm, the height is 1-1.5 cm, the groove 13 at the upper part of the container 1 is surrounded by 2 concave arc surfaces, and the length of the groove 13 is 1-3 cm, the width is 0.5-2 cm, and the depth is 0.4-0.7 cm.
(4) Multimode As2S3Fixing and protecting chalcogenide glass bare optical fiber
Fixing the bare optical fiber obtained in the step (2) on an optical fiber clamp, and pressing two ends of the bare optical fiber through the optical fiber clamp, wherein the optical fiber clamp adopts the prior art, and a clamping plate of the optical fiber clamp is attracted under the action of magnetic force and presses the optical fiber through a soft rubber strip; a three-dimensional optical adjusting frame (not shown in the figure) is placed below the bare optical fiber, the container 1 is placed at the top of the three-dimensional optical adjusting frame, the distance between the optical fiber clamp and the container 1 is adjusted through the three-dimensional optical adjusting frame, so that two sides of the bare optical fiber are respectively embedded into the first positioning groove 11 and the second positioning groove 12, and the middle part of the bare optical fiber is positioned in the groove 13;
(5) multimode As2S3Chemical corrosion of chalcogenide glass bare fiber
Pouring the sodium hydroxide solution prepared in the step (1) into an alkali solution supply unit, starting the alkali solution supply unit, continuously introducing the sodium hydroxide solution into a guide solution channel, keeping the liquid level of the sodium hydroxide solution in the groove 13 above the upper surface of the bare fiber, chemically corroding the surface of the middle part of the bare fiber through the sodium hydroxide solution in the groove 13, observing the outer diameter of the bare fiber in real time through a CCD camera, slowly raising the glass slide through a three-dimensional optical adjusting frame to ensure that the upper surface of the glass slide just contacts with the lower surface of the bare fiber when the environmental temperature during chemical corrosion is 28 ℃ and the outer diameter of the bare fiber reaches a preset value after the chemical corrosion is about 4min, closing the alkali solution supply unit, removing the container 1, placing a glass slide (not shown in the figure) at the top of the three-dimensional optical adjusting frame, fixing two ends of the bare fiber on the glass slide, finally cleaning the surface of the bare fiber by deionized water, drying to obtain the multimode As2S3The cross-sectional photograph of the tapered region of the chalcogenide glass tapered optical fiber is shown in FIG. 3, and the lengthwise appearance photograph of the tapered region is shown in FIG. 4. The multimode As2S3The outer diameter of the cladding of the chalcogenide glass tapered fiber was 62 μm, and the outer diameter of the core was kept at 61 μm.
For multimode As in example 12S3The chalcogenide glass tapered optical fiber adopts the method of the invention, and measures the multimode As corresponding to different chemical corrosion times under the mass concentration by keeping the mass concentration of 4 percent of sodium hydroxide solution unchanged2S3The change of the outer diameter of the chalcogenide glass tapered optical fiber cladding establishes multimode As2S3The corrosion time-cladding diameter curve for chalcogenide glass tapered fibers is shown in FIG. 5.
Example 2: in multiple modes of Ge10As24S66The chalcogenide glass tapered optical fiber is taken as an example, and the multimode Ge is prepared by adopting the chemical corrosion preparation method of the invention10As24S66The chalcogenide glass tapered optical fiber was prepared in substantially the same manner as in example 1 except that in example 2, the quality of the sodium hydroxide solution used for chemical etching was changedThe concentration is 10%, and the chemical etching time is 2 min. Before chemical etching, multimode Ge10As24S66The chalcogenide glass had a cladding outer diameter of 237 μm and a core outer diameter of 58 μm. Chemically etching for 2min to obtain multi-mode Ge10As24S66The outer diameter of the cladding of the chalcogenide glass tapered fiber was 60 μm, and the outer diameter of the core was kept at 58 μm. The multimode Ge is10As24S66The cross-sectional photograph of the tapered region of the chalcogenide glass tapered fiber is shown in FIG. 6, and the lengthwise appearance photograph of the tapered region is shown in FIG. 7.
For multimode Ge in example 210As24S66The chalcogenide glass tapered optical fiber adopts the method of the invention, and measures the multimode Ge corresponding to sodium hydroxide solution with different mass concentrations under the corrosion time with the chemical corrosion time of 2min unchanged10As24S66The change of the outer diameter of the chalcogenide glass tapered optical fiber cladding establishes multimode Ge10As24S66The sodium hydroxide solution concentration-cladding diameter curve of chalcogenide glass tapered fiber is shown in FIG. 8.
Example 3: as in a single mode2S3The chalcogenide glass tapered optical fiber is taken As an example, and the single-mode As is prepared by the chemical corrosion preparation method of the invention2S3The chalcogenide glass tapered optical fiber was prepared in substantially the same manner as in example 1, except that in example 2, the sodium hydroxide solution used for chemical etching had a mass concentration of 4% and the chemical etching time was 2.5 min. Single mode As before chemical etching2S3The chalcogenide glass had a cladding outer diameter of 217 μm and a core outer diameter of 13 μm. Chemically etching for 2.5min to obtain single-mode As2S3The outer diameter of the cladding of the chalcogenide glass tapered fiber was 30 μm, and the outer diameter of the core was kept at 13 μm.
Example 4: in multiple modes of As2Se3The chalcogenide glass tapered optical fiber is taken As an example, and the multimode As is prepared by adopting the chemical corrosion preparation method of the invention2Se3The chalcogenide glass tapered optical fiber was prepared in substantially the same manner as in example 1, except that in example 2, the sodium hydroxide solution used for the chemical etching had a mass concentration of 4% and the chemical etching time was set to be shortIs 2 min. Before chemical etching, multimode As2Se3The chalcogenide glass had a cladding outer diameter of 219 μm and a core outer diameter of 38 μm. Chemical etching for 2min to obtain multimode As2Se3The chalcogenide glass tapered fiber had a cladding outer diameter of 44 μm and a core outer diameter of 38 μm.
Claims (5)
1. A chemical corrosion preparation method of chalcogenide glass tapered optical fiber is characterized by comprising the following steps:
(1) preparing sodium hydroxide solution
Preparing a proper amount of sodium hydroxide solution with a certain concentration, and cooling to room temperature for later use;
(2) removal of chalcogenide glass optical fiber coating
Preparing a chalcogenide glass optical fiber, wherein the structure of the chalcogenide glass optical fiber comprises a fiber core, a cladding and a coating layer, the fiber core and the cladding are both made of chalcogenide glass, and the coating layer is a high polymer layer;
intercepting a section of chalcogenide glass optical fiber, soaking the chalcogenide glass optical fiber in dimethylacetamide, removing a coating layer on the surface of the chalcogenide glass optical fiber to obtain a bare fiber, soaking the bare fiber in alcohol, washing off the dimethylacetamide remaining on the surface of the bare fiber, taking out the bare fiber, and wiping and cleaning the surface of the bare fiber for later use;
(3) preparation of etching apparatus
Preparing a corrosion device, wherein the corrosion device comprises a container, an alkali liquor supply unit and an alkali liquor collection unit, a liquid guide channel is arranged in the container, a first concave positioning groove, a second concave positioning groove and a groove which penetrate through the container in the length direction are arranged at the upper part of the container, the groove is communicated with the liquid guide channel up and down, the width of the groove is larger than the outer diameter of the liquid guide channel, the length of the groove is matched with the length of a conical area of a conical optical fiber to be prepared, the first positioning groove and the second positioning groove are respectively arranged at two sides of the groove and are respectively communicated with the groove horizontally, the axis of the first positioning groove and the axis of the second positioning groove are on the same straight line, and the connecting line of the axis of the first positioning groove and the axis of the second positioning groove transversely penetrates through the groove, the widths of the first positioning groove and the second positioning groove are respectively matched with the outer diameter of the bare optical fiber, the liquid outlet of the alkali liquor supply unit is communicated with one end of the liquid guide channel, and the other end of the liquid guide channel is communicated with the liquid inlet of the alkali liquor collection unit; the alkali liquor supply unit is used for continuously introducing a sodium hydroxide solution into the liquid guide channel, and the alkali liquor collection unit is used for collecting the sodium hydroxide solution discharged from the liquid guide channel; a CCD camera connected with a computer is suspended above the container, and a lens of the CCD camera faces downwards and is opposite to the groove;
(4) fixing and protecting chalcogenide glass bare optical fiber
Fixing the bare optical fiber obtained in the step (2) on an optical fiber clamp, tightly pressing two ends of the bare optical fiber through the optical fiber clamp, placing a three-dimensional optical adjusting frame below the bare optical fiber, placing the container on the top of the three-dimensional optical adjusting frame, adjusting the distance between the optical fiber clamp and the container through the three-dimensional optical adjusting frame, respectively embedding two sides of the bare optical fiber into the first positioning groove and the second positioning groove, and enabling the middle part of the bare optical fiber to be positioned in the groove;
(5) chemical corrosion of chalcogenide glass bare fiber
Pouring the sodium hydroxide solution prepared in the step (1) into the alkali liquor supply unit, starting the alkali liquor supply unit, continuously introducing the sodium hydroxide solution into the liquid guide channel, keeping the liquid level of the sodium hydroxide solution in the groove above the upper surface of the bare fiber, the surface of the middle part of the bare fiber is chemically corroded by the sodium hydroxide solution in the groove, the outer diameter of the bare fiber is observed in real time by a CCD camera, when the outer diameter of the bare fiber reaches a predetermined value, the alkali supply unit is closed, the container is removed, a glass slide is placed on the top of the three-dimensional optical adjusting frame, the glass slide is slowly lifted through the three-dimensional optical adjusting frame, so that the upper surface of the glass slide just contacts with the lower surface of the bare fiber, and fixing two ends of the bare fiber on a glass slide, finally cleaning the surface of the bare fiber by using deionized water and alcohol, and drying to obtain the chalcogenide glass tapered fiber.
2. The chemical corrosion preparation method of the chalcogenide glass tapered optical fiber according to claim 1, wherein the mass concentration of the sodium hydroxide solution prepared in the step (1) is 2-10%, and the corrosion time of the surface of the middle part of the bare optical fiber in the step (5) is 2-5 min.
3. The method of claim 1, wherein in step (2), the chalcogenide glass optical fiber is As2S3、As2Se3Ge-As-Se or Ge-As-S chalcogenide glass fibers.
4. The chemical etching method for preparing chalcogenide glass tapered optical fiber according to claim 1, wherein the outer diameter of the cladding in step (2) is 150 to 300 μm, and the outer diameter of the core is 10 to 100 μm.
5. The method for preparing chalcogenide glass tapered optical fiber according to claim 1, wherein the environment temperature for performing the chemical etching in the step (5) is 25 to 50 ℃.
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| CN113664667A (en) * | 2021-08-19 | 2021-11-19 | 宁波大学 | Side polishing method of chalcogenide glass optical fiber |
| CN113860727A (en) * | 2021-08-27 | 2021-12-31 | 哈尔滨工程大学 | Preparation method of self-deformation core optical fiber based on oxyhydrogen flame heating |
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| CN113860727A (en) * | 2021-08-27 | 2021-12-31 | 哈尔滨工程大学 | Preparation method of self-deformation core optical fiber based on oxyhydrogen flame heating |
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Application publication date: 20200501 |