Fluorine indium-based glass optical fiber and preparation method thereof

Abstract

The invention belongs to the technical field of fluorine indium-based glass optical fibers, and particularly relates to a fluorine indium-based glass optical fiber and a preparation method thereof. The method comprises the following steps: firstly, sleeving a prepared fluorine indium-based glass preform with a polyether-ether-ketone sleeve, and vacuumizing a gap between the polyether-ether-ketone sleeve and the fluorine indium-based glass preform; heating the bottoms of the polyether-ether-ketone sleeve and the fluorine-indium-based glass preform, so that the polyether-ether-ketone sleeve is heated to wrap the fluorine-indium-based glass preform to form an optical fiber preform; and performing wire drawing treatment on the optical fiber preform to obtain the high-performance fluorine indium-based glass optical fiber. The fluorine-indium-based glass optical fiber prepared by wrapping the fluorine-indium-based glass preform with the polyether-ether-ketone has the characteristics of low loss, excellent bending resistance and the like, and the whole preparation process is simple and environment-friendly and is suitable for industrial production.

Description

Technical Field

[0001] The invention belongs to the technical field of fluorine-indium-based glass optical fibers, and in particular relates to a fluorine-indium-based glass optical fiber and a preparation method thereof. Background Art

[0002] Fluorine-indium-based glass optical fiber has extremely high light transmittance in the visible to mid-infrared band. It is the most promising ultra-low-loss optical fiber material for long-distance base station-free communication and has become a strategic key technology in the competition among major countries. Therefore, the preparation of high-performance fluorine-indium-based glass optical fiber is crucial.

[0003] The preparation process of fluorine-indium-based glass optical fiber is mainly as follows: first, a fluorine-indium-based glass preform is prepared, and then the fluorine-indium-based glass preform is subjected to a drawing process to obtain a fluorine-indium-based glass optical fiber. However, when drawing fluorine-indium-based glass optical fiber, due to its poor glass-forming properties, it is very easy to crystallize during the drawing process, resulting in increased fiber loss and decreased mechanical properties. In addition, the large surface tension of the fluorine-indium-based glass preform is also an important reason for the easy crystallization during the drawing process. Therefore, it is necessary to add a coating material to the outside of the fluorine-indium-based glass preform before the drawing process. Polytetrafluoroethylene (PTFE) is the most commonly considered material and has been successfully used in fluorine-zirconium-based glass optical fibers. In view of the high glass transition temperature of fluorine-indium glass, polytetrafluoroethylene is not perfectly suitable for fluorine-indium-based glass optical fibers.

[0004] Therefore, the prior art still needs to be improved and developed. Summary of the invention

[0005] In order to solve the above problems, the purpose of the present invention is to provide a method for preparing high-performance fluorine-indium-based glass optical fiber by wrapping a fluorine-indium-based glass preform rod with polyetheretherketone (PEEK), aiming to solve the technical problem that polytetrafluoroethylene cannot be perfectly adapted to fluorine-indium-based glass optical fiber due to the high glass transition temperature of fluorine-indium-based glass.

[0006] The technical solution of the present invention is as follows:

[0007] A first aspect of the present invention provides a method for preparing a fluorine-indium-based glass optical fiber, comprising:

[0008] Step 1, putting a polyetheretherketone sleeve on the prepared fluorine-indium-based glass preform rod, and performing a vacuum treatment on the gap between the polyetheretherketone sleeve and the fluorine-indium-based glass preform rod;

[0009] Step 2, after the vacuum treatment is completed, the polyetheretherketone sleeve and the bottom of the fluorine-indium-based glass preform rod are heated so that the polyetheretherketone sleeve is heated to wrap the fluorine-indium-based glass preform rod to form an optical fiber preform, and then the optical fiber preform is drawn to obtain a high-performance fluorine-indium-based glass optical fiber.

[0010] Optionally, in step 1, the composition of the fluorine-indium-based glass preform includes InF3, BaF2, SrF2, ZnF2, GaF3, NaF, LiF and YF3;

[0011] Alternatively, the composition of the fluorine-indium-based glass preform includes InF3, BaF2, SrF2, ZnF2, GaF3, NaF, LiF, YF3 and PbF2.

[0012] Optionally, in step 1, the fluorine-indium-based glass preform has a diameter of 12 to 15 mm and a length of 100 to 150 mm.

[0013] Optionally, the softening temperature of the polyetheretherketone sleeve is 300-350°C.

[0014] Optionally, in step 1, the thickness of the polyetheretherketone sleeve is 1 mm.

[0015] Optionally, in step 1, the vacuum treatment refers to reducing the vacuum degree to below 0.1 Pa.

[0016] Optionally, in step 2, the heating temperature of the heating treatment is 300-350°C.

[0017] Optionally, the step 1 specifically includes:

[0018] After the prepared fluorine-indium-based glass preform is covered with a polyetheretherketone sleeve, it is placed in a quartz tube with a heating device, and the gap between the polyetheretherketone sleeve and the fluorine-indium-based glass preform is evacuated until the vacuum degree drops below 0.1Pa.

[0019] Optionally, the step 2 specifically includes:

[0020] After the vacuum treatment is completed, the heating device is started to heat the polyetheretherketone sleeve and the bottom of the fluorine-indium-based glass preform rod to 300-350° C. After being heated, the polyetheretherketone sleeve automatically wraps the fluorine-indium-based glass preform rod to become an optical fiber preform, and then a drawing tower is used to draw the optical fiber preform into a fluorine-indium-based glass optical fiber.

[0021] A second aspect of the present invention provides a fluorine-indium-based glass optical fiber, wherein the fluorine-indium-based glass optical fiber is prepared using the preparation method of the fluorine-indium-based glass optical fiber described in the present invention.

[0022] Compared with the prior art, the advantages of the present invention are:

[0023] The glass-forming properties of fluorine-indium-based glass optical fibers are poor, and the surface tension of fluorine-indium-based glass preforms is large, which makes it very easy to crystallize during the process of drawing into optical fibers. Therefore, adding a suitable coating material before drawing is a good choice, which can effectively reduce the risk of crystallization of fluorine-indium-based glass optical fibers. The selected coating material polyetheretherketone has physical and chemical properties such as high temperature resistance and chemical corrosion resistance. The most important thing is that the transition temperatures of polyetheretherketone and fluorine-indium-based glass have very good adaptability, and can better match fluorine-indium-based glass compared to other materials such as polytetrafluoroethylene. In addition, the vacuum treatment can make polyetheretherketone wrap the fluorine-indium-based glass preform at a lower temperature, further reducing the risk of crystallization. The fluorine-indium-based glass optical fiber prepared by polyetheretherketone wrapping the fluorine-indium-based glass preform of the present invention has the characteristics of low loss and excellent bending resistance. The entire preparation process is simple, environmentally friendly, safe and convenient, efficient and easy to control, and suitable for industrial production. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 A partial schematic diagram of an apparatus for preparing fluorine-indium-based glass optical fiber provided in an embodiment of the present invention. DETAILED DESCRIPTION

[0025] In order to make the purpose, technical solution and advantages of the embodiments of the present application clearer, the technical solution in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of this application.

[0026] An embodiment of the present invention provides a method for preparing a fluorine-indium-based glass optical fiber, comprising:

[0027] Step 1, putting a polyetheretherketone sleeve on the prepared fluorine-indium-based glass preform rod, and performing a vacuum treatment on the gap between the polyetheretherketone sleeve and the fluorine-indium-based glass preform rod;

[0028] Step 2, after the vacuum treatment is completed, the polyetheretherketone sleeve and the bottom of the fluorine-indium-based glass preform rod are heated so that the polyetheretherketone sleeve is heated to wrap the fluorine-indium-based glass preform rod to form an optical fiber preform, and then the optical fiber preform is drawn to obtain a high-performance fluorine-indium-based glass optical fiber.

[0029] The main components of fluorine-indium-based glass are InF3-ZnF2-BaF2-SrF2-GaF3. In addition, a small amount of YF3, LaF3, PbF2, LiF, NaF and other substances are doped to improve the glass-forming properties. The transition temperatures of these fluorine-indium-based glasses are mostly around 250-300°C. In this temperature range, polyetheretherketone can provide a matching softening temperature. In addition, polyetheretherketone also has physical and chemical properties such as high temperature resistance and chemical corrosion resistance. It is an ideal optical fiber wrapping material and can provide good protection for optical fibers. Therefore, an embodiment of the present invention provides a method for preparing high-performance fluorine-indium-based glass optical fibers by wrapping fluorine-indium-based glass preforms with polyetheretherketone. Specifically, a polyetheretherketone casing is added to the outside of the fluorine-indium-based glass preform, and then vacuumized and locally heated, so that a high-performance fluorine-indium-based glass optical fiber can be drawn. The fluorine-indium-based glass optical fiber prepared by wrapping a fluorine-indium-based glass preform rod with polyetheretherketone in the embodiment of the present invention has the characteristics of low loss and excellent bending resistance. The entire preparation process is simple, environmentally friendly, safe, convenient, efficient, easy to control, and suitable for industrial production.

[0030] In one embodiment, in step 1, the softening temperature of the polyetheretherketone sleeve is 300-350°C, such as 300°C, 310°C, 320°C, 330°C, 340°C or 350°C, etc. The transition temperature of polyetheretherketone and fluorine-indium-based glass at this softening temperature has better compatibility, so that polyetheretherketone can better match fluorine-indium-based glass.

[0031] In one embodiment, in step 1, the thickness of the polyetheretherketone sleeve is 1 mm. By using a polyetheretherketone sleeve of this thickness to wrap the fluorine-indium-based glass preform rod, the risk of crystallization of the fluorine-indium-based glass optical fiber can be minimized and the optical fiber loss can be reduced.

[0032] In one embodiment, in step 1, the composition of the fluorine-indium-based glass preform includes InF3, BaF2, SrF2, ZnF2, GaF3, NaF, LiF and YF3;

[0033] Alternatively, the composition of the fluorine-indium-based glass preform includes InF3, BaF2, SrF2, ZnF2, GaF3, NaF, LiF, YF3 and PbF2.

[0034] Preferably, the fluorine-indium-based glass preform consists of InF3, BaF2, SrF2, ZnF2, GaF3, NaF, LiF and YF3, which is recorded as InF3-BaF2-SrF2-ZnF2-GaF3-NaF-LiF-YF3.

[0035] The above composition can improve the glass forming performance. The transition temperature of the fluorine-indium-based glass of this composition is about 250-300° C., and polyetheretherketone can provide a matching softening temperature in this temperature range.

[0036] More preferably, the components and molar ratio of the fluorine-indium-based glass preform are 25.5InF3-18BaF2-8SrF2-15ZnF2-11.5GaF3-12NaF-5LiF-5YF3.

[0037] By adopting the above composition, the glass-forming properties can be further improved, and polyetheretherketone can provide a more matching softening temperature.

[0038] Preferably, the fluorine-indium-based glass preform is composed of InF3, BaF2, SrF2, ZnF2, GaF3, NaF, LiF, YF3 and PbF2, denoted as

[0039] InF3-BaF2-SrF2-ZnF2-GaF3-NaF-LiF-YF3-PbF2.

[0040] The above composition can improve the glass forming performance. The transition temperature of the fluorine-indium-based glass of this composition is about 250° C. to 300° C., and polyetheretherketone can provide a matching softening temperature in this temperature range.

[0041] More preferably, the components and molar ratio of the fluorine-indium-based glass preform are 25.5InF3-18BaF2-8SrF2-15ZnF2-11.5GaF3-7NaF-5LiF-5YF3-5PbF2.

[0042] By adopting the above composition, the glass-forming properties can be further improved, and polyetheretherketone can provide a more matching softening temperature.

[0043] In one embodiment, in step 1, the fluorine-indium-based glass preform has a diameter of 12 to 15 mm and a length of 100 to 150 mm.

[0044] Preferably, the fluorine-indium-based glass preform has a diameter of 12 mm and a length of 100 mm, which is expressed as Φ12 mm×100 mm.

[0045] In one embodiment, in step 1, the vacuum treatment refers to reducing the vacuum degree to below 0.1 Pa, such as 0.05 Pa, 0.01 Pa, etc. Under this condition, it can be ensured that the polyetheretherketone wraps the fluorine-indium-based glass preform at a lower temperature, further reducing the risk of crystallization and reducing optical fiber loss.

[0046] In one embodiment, in step 2, the heating temperature of the heat treatment is 300-350° C. This is because the transition temperature of fluorine-indium-based glass is around 250-300° C., so the heating temperature is selected to be 300-350° C. In this heating temperature range, polyetheretherketone can soften.

[0047] In one embodiment, the step 1 specifically includes:

[0048] like Figure 1 As shown, after the prepared fluorine-indium-based glass preform is covered with a polyetheretherketone sleeve, it is placed in a quartz tube with a heating device, and the gap between the polyetheretherketone sleeve and the fluorine-indium-based glass preform is evacuated until the vacuum degree drops below 0.1Pa.

[0049] In one embodiment, the step 2 specifically includes:

[0050] After the vacuum treatment is completed, the heating device is started to heat the polyetheretherketone sleeve and the bottom of the fluorine-indium-based glass preform rod (see Figure 1 The fiber optic preform is then drawn into a fluorine-indium-based glass optical fiber using a drawing tower.

[0051] An embodiment of the present invention provides a fluorine-indium-based glass optical fiber, wherein the fluorine-indium-based glass optical fiber is prepared using the preparation method of the fluorine-indium-based glass optical fiber described in the embodiment of the present invention.

[0052] The fluorine-indium-based glass optical fiber prepared by wrapping a fluorine-indium-based glass preform rod with polyetheretherketone has the characteristics of low loss, excellent bending resistance and the like.

[0053] The present invention is further described in detail below through several embodiments.

[0054] Example 1

[0055] (1) Preparation of fluorine-indium-based glass preform: The fluorine-indium-based glass components and their molar ratios are 25.5InF3-18BaF2-8SrF2-15ZnF2-11.5GaF3-12NaF-5LiF-5YF3, which are melted at 900°C for 2 hours in a CF4 atmosphere and poured into a mold to form a fluorine-indium-based glass preform with a diameter of 12 mm and a length of 100 mm;

[0056] (2) Wrapping the preform rod with a polyetheretherketone sleeve: Place the fluorine-indium-based glass preform rod into a polyetheretherketone sleeve with a thickness of 1 mm, and place it in a quartz tube with a heating device. Evacuate the gap between the polyetheretherketone sleeve and the fluorine-indium-based glass preform rod, and when the vacuum degree drops to 0.05 Pa, start the heating device to heat the polyetheretherketone sleeve and the bottom of the fluorine-indium-based glass preform rod to 300°C. After being heated, the polyetheretherketone sleeve automatically wraps the fluorine-indium-based glass preform rod to become an optical fiber preform;

[0057] (3) Drawing an optical fiber preform: Using a drawing tower, the optical fiber preform is drawn into a fluorine-indium-based glass optical fiber.

[0058] Example 2

[0059] (1) Preparation of fluorine-indium-based glass preform: The fluorine-indium-based glass components and their molar ratios are 25.5InF3-18BaF2-8SrF2-15ZnF2-11.5GaF3-7NaF-5LiF-5YF3-5PbF2. They are melted at 900°C for 2 hours in a CF4 atmosphere and poured into a mold to form a fluorine-indium-based glass preform with a diameter of 12 mm and a length of 100 mm.

[0060] (2) Wrapping the preform rod with a polyetheretherketone sleeve: Place the fluorine-indium-based glass preform rod into a polyetheretherketone sleeve with a thickness of 1 mm, and place it in a quartz tube with a heating device. Evacuate the gap between the polyetheretherketone sleeve and the fluorine-indium-based glass preform rod, and when the vacuum degree drops to 0.05 Pa, start the heating device to heat the polyetheretherketone sleeve and the bottom of the fluorine-indium-based glass preform rod to 350°C. After being heated, the polyetheretherketone sleeve automatically wraps the fluorine-indium-based glass preform rod to become an optical fiber preform;

[0061] (3) Drawing an optical fiber preform: Using a drawing tower, the optical fiber preform is drawn into a fluorine-indium-based glass optical fiber.

[0062] Example 3

[0063] (1) Preparation of fluorine-indium-based glass preform: The fluorine-indium-based glass components and their molar ratios are 25.5InF3-18BaF2-8SrF2-15ZnF2-11.5GaF3-7NaF-5LiF-5YF3-5PbF2. They are melted at 900°C for 2 hours in a CF4 atmosphere and poured into a mold to form a fluorine-indium-based glass preform with a diameter of 12 mm and a length of 100 mm.

[0064] (2) Wrapping the preform rod with a polyetheretherketone sleeve: Place the fluorine-indium-based glass preform rod into a polyetheretherketone sleeve with a thickness of 1 mm, and place it in a quartz tube with a heating device. Evacuate the gap between the polyetheretherketone sleeve and the fluorine-indium-based glass preform rod, and when the vacuum degree drops to 0.01 Pa, start the heating device to heat the polyetheretherketone sleeve and the bottom of the preform rod to 300°C. After being heated, the polyetheretherketone sleeve automatically wraps the fluorine-indium-based glass preform rod to become an optical fiber preform;

[0065] (3) Drawing an optical fiber preform: Using a drawing tower, the optical fiber preform is drawn into a fluorine-indium-based glass optical fiber.

[0066] Comparative Example 1

[0067] The other steps are the same as those in Example 1, except that the sleeve material is polytetrafluoroethylene (PTFE).

[0068] Comparative Example 2

[0069] The other steps are the same as those in Example 2, except that the sleeve material is polytetrafluoroethylene (PTFE).

[0070] Comparative Example 3

[0071] The other steps are the same as those in Example 3, except that the sleeve material is polytetrafluoroethylene (PTFE).

[0072] The losses of the fluorine-indium-based glass optical fibers prepared in the above three embodiments are shown in Table 1 below:

[0073] Table 1

[0074] Loss(Db / km) Example 1 54 Example 2 47 Example 3 33 Comparative Example 1 257 Comparative Example 2 211 Comparative Example 3 189

[0075] It can be seen from Table 1 that compared with the traditional sheath material polytetrafluoroethylene, the fluorine-indium-based glass optical fiber drawn from the polyetheretherketone sheath has lower loss.

[0076] In summary, the present invention provides a fluorine-indium-based glass optical fiber and a preparation method thereof. The coating material polyetheretherketone selected by the present invention has physical and chemical properties such as high temperature resistance and chemical corrosion resistance, and can better match the transition temperature of fluorine-indium-based glass compared to polytetrafluoroethylene. In addition, the vacuum treatment can allow polyetheretherketone to wrap the fluorine-indium-based glass preform at a lower temperature, further reducing the risk of crystallization. The fluorine-indium-based glass optical fiber prepared by wrapping the fluorine-indium-based glass preform with polyetheretherketone in the present invention has the characteristics of low loss and excellent bending resistance. The entire preparation process is simple, environmentally friendly, safe and convenient, efficient and easy to control, and suitable for industrial production.

[0077] The above description is only a specific implementation of the present application, so that those skilled in the art can understand or implement the present application. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application will not be limited to the embodiments shown herein, but will conform to the widest range consistent with the principles and novel features applied for herein.

Claims

1. A method for preparing a fluorine-indium-based glass optical fiber, characterized in that: include: Step 1, putting a polyetheretherketone sleeve on the prepared fluorine-indium-based glass preform rod, and performing a vacuum treatment on the gap between the polyetheretherketone sleeve and the fluorine-indium-based glass preform rod; Step 2, after the vacuum treatment is completed, the polyetheretherketone sleeve and the bottom of the fluorine-indium-based glass preform rod are heated so that the polyetheretherketone sleeve is heated to wrap the fluorine-indium-based glass preform rod to form an optical fiber preform, and then the optical fiber preform is drawn to obtain a fluorine-indium-based glass optical fiber.

2. The method for preparing the fluorine-indium-based glass optical fiber according to claim 1, characterized in that: In the step 1, the composition of the fluorine-indium-based glass preform includes InF3, BaF2, SrF2, ZnF2, GaF3, NaF, LiF and YF3; Alternatively, the composition of the fluorine-indium-based glass preform includes InF3, BaF2, SrF2, ZnF2, GaF3, NaF, LiF, YF3 and PbF2.

3. The method for preparing the fluorine-indium-based glass optical fiber according to claim 1, characterized in that: In the step 1, the diameter of the fluorine-indium-based glass preform is 12-15 mm and the length is 100-150 mm.

4. The method for preparing the fluorine-indium-based glass optical fiber according to claim 1, characterized in that: In the step 1, the softening temperature of the polyetheretherketone sleeve is 300-350°C.

5. The method for preparing fluorine-indium-based glass optical fiber according to claim 1, characterized in that: In the step 1, the thickness of the polyetheretherketone sleeve is 1 mm.

6. The method for preparing fluorine-indium-based glass optical fiber according to claim 1, characterized in that: In the step 1, the vacuum treatment refers to reducing the vacuum degree to below 0.1 Pa.

7. The method for preparing fluorine-indium-based glass optical fiber according to claim 1, characterized in that: In the step 2, the heating temperature of the heating treatment is 300-350°C.

8. The method for preparing fluorine-indium-based glass optical fiber according to claim 1, characterized in that: The step 1 specifically includes: After the prepared fluorine-indium-based glass preform is covered with a polyetheretherketone sleeve, it is placed in a quartz tube with a heating device, and the gap between the polyetheretherketone sleeve and the fluorine-indium-based glass preform is evacuated until the vacuum degree drops below 0.1Pa.

9. The method for preparing fluorine-indium-based glass optical fiber according to claim 8, characterized in that: The step 2 specifically includes: After the vacuum treatment is completed, the heating device is started to heat the polyetheretherketone sleeve and the bottom of the fluorine-indium-based glass preform rod to 300-350° C. After being heated, the polyetheretherketone sleeve automatically wraps the fluorine-indium-based glass preform rod to become an optical fiber preform, and then a drawing tower is used to draw the optical fiber preform into a fluorine-indium-based glass optical fiber.

10. A fluorine-indium-based glass optical fiber, characterized in that: The fluorine-indium-based glass optical fiber is prepared by the preparation method of any one of claims 1 to 9.

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