Special polishing solution for fluoride glass as well as preparation method and application of special polishing solution

Abstract

The invention belongs to the field of fluoride glass polishing, and particularly relates to a special polishing solution for fluoride glass as well as a preparation method and application thereof. The polishing solution comprises cerium oxide (CeO2), zirconium oxychloride (ZrOCl2) and water (H2O), the concentration of the cerium oxide is 1-5 g / mL, and the concentration of the zirconium oxychloride is 0.1-1 mol / L. On the basis of a conventional polishing solution, by adding a proper amount of zirconium oxychloride, generation of hydroxide and fluorine hydroxide on the surface of fluoride glass can be reduced, and the surface roughness of the fluoride glass is reduced, so that the surface polishing quality of a fluoride glass preform rod is effectively improved, and the crystallization phenomenon in the subsequent optical fiber drawing process is reduced; and fiber loss is reduced.

Description

Technical Field

[0001] The invention belongs to the field of fluoride glass polishing, and in particular relates to a special polishing liquid for fluoride glass and a preparation method and application thereof. Background Art

[0002] Fluoride optical fiber, as an important material for mid-infrared lasers, has the advantages of high rare earth solubility, relatively low phonon energy, wide optical window, low reflectivity, low dispersion and easy processing and manufacturing. In recent years, it has been widely used in military, communications, medicine, environmental science and other fields, and has become a strategic key technology in the competition among major powers.

[0003] Fluoride optical fiber is an optical fiber made of fluoride glass. Specifically, fluoride glass is first made into a fluoride glass preform rod, and then the fluoride glass preform rod is drawn into a fluoride optical fiber. However, fluoride glass has some disadvantages. The chemical stability of its surface is poor and it is easily corroded by water molecules. In an aqueous solution or a water-containing environment, the surface is prone to generate insoluble hydroxides and fluoride hydroxides and form a hydration layer, which causes the fluoride glass to lose transparency. The main methods for preparing fluoride glass preform rods are the sleeve method, the extrusion method and the casting method, among which the sleeve method is currently the most widely used method. This method belongs to optical cold processing, which will leave ionic impurities on the surface and produce micro-defects such as microcracks on the sub-surface. Fluoride glass preform rods processed by conventional polishing liquid (usually prepared by water and cerium oxide polishing powder) are prone to crystallization or devitrification when drawing optical fiber, which increases optical fiber loss and reduces the mechanical properties of optical fiber.

[0004] Therefore, the improvement of fluoride glass polishing process is urgent. Summary of the invention

[0005] In order to solve the above problems, the purpose of the present invention is to provide a special polishing liquid for fluoride glass and its preparation method and application, aiming to solve the problem of crystallization and increased loss of fluoride glass preform rods processed by conventional polishing liquid during subsequent optical fiber drawing.

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

[0007] In a first aspect of the present invention, a polishing liquid specifically for fluoride glass is provided, wherein the polishing liquid comprises cerium oxide (CeO2), zirconium oxychloride (ZrOCl2) and water (H2O), the concentration of the cerium oxide is 1 to 5 g / mL, and the concentration of the zirconium oxychloride is 0.1 to 1 mol / L.

[0008] Optionally, every 500 mL of the polishing liquid is prepared by adding 500 to 2500 grams of cerium oxide powder and 16 to 160 grams of zirconium oxychloride octahydrate powder into deionized water and mixing.

[0009] Optionally, the particle size of the cerium oxide powder is 100-300 nanometers.

[0010] The second aspect of the present invention provides a method for preparing a special polishing liquid for fluoride glass, which comprises the steps of: mixing cerium oxide, zirconium oxychloride and water to obtain a polishing liquid; wherein the concentration of the cerium oxide is 1 to 5 g / mL, and the concentration of the zirconium oxychloride is 0.1 to 1 mol / L.

[0011] Optionally, the method specifically includes the steps of:

[0012] Step 1, weighing 500-2500 g of cerium oxide powder and 16-160 g of zirconium oxychloride octahydrate powder;

[0013] Step 2: add deionized water to the weighed cerium oxide powder and zirconium oxychloride octahydrate powder, mix, and dilute to 500 mL to obtain the polishing liquid.

[0014] Optionally, the particle size of the cerium oxide powder is 100-300 nanometers.

[0015] The third aspect of the present invention provides a fluoride glass-specific polishing liquid according to the present invention for use in polishing fluoride glass.

[0016] Optionally, the composition of the fluoride glass includes InF3, BaF2, SrF2, ZnF2, GaF3, NaF, LiF and YF3;

[0017] Alternatively, the composition of the fluoride glass includes InF3, BaF2, SrF2, ZnF2, GaF3, NaF, LiF, YF3 and PbF2;

[0018] Alternatively, the composition of the fluoride glass includes ZrF4, BaF2, LaF3, AlF3 and NaF;

[0019] Alternatively, the composition of the fluoride glass includes ZrF4, BaF2, LaF3, AlF3, NaF and PbF2.

[0020] Optionally, the application method comprises the steps of:

[0021] Fluoride glass is available;

[0022] Making the fluoride glass into a fluoride glass preform;

[0023] After rough grinding and fine grinding of the fluoride glass preform, the fluoride glass preform is polished using the polishing liquid;

[0024] The polished fluoride glass preform is drawn into a fluoride optical fiber using a drawing tower.

[0025] Compared with the prior art, the advantages of the present invention are:

[0026] The present invention reduces the generation of hydroxide and fluoride hydroxide on the surface of fluoride glass and reduces the surface roughness of fluoride glass by adding an appropriate amount of zirconium dichloride (ZrOCl2) to a conventional polishing liquid (formed by cerium oxide and water), thereby effectively improving the surface polishing quality of fluoride glass preform rods, reducing the crystallization phenomenon in the subsequent optical fiber drawing process, and reducing optical fiber loss.

[0027] This is because during the polishing process of fluoride glass, fluoride and water will react to form insoluble hydroxides and produce fluoride ions in the liquid boundary layer. When the fluoride ions exceed the solubility product, a reverse reaction of hydrolysis will occur, forming a fluoride precipitate with a smaller solubility product. In this way, a precipitation layer of hydroxide and fluoride will form on the originally uniform surface of the fluoride glass, resulting in crystallization and increased loss in the subsequent optical fiber drawing process. By introducing zirconium dichloride (ZrOCl2) into conventional polishing liquid, ZrO in the solution 2+ Can be used as a complexing agent for fluoride ions to generate ZrOF4 2- , hindering the formation of fluoride precipitation in the glass surface layer.

[0028] In addition, the product of the present invention is not only simple to prepare and green and environmentally friendly, but also can effectively reduce the crystallization phenomenon on the surface of fluoride glass and reduce optical fiber loss when applied to fluoride glass polishing. DETAILED DESCRIPTION

[0029] 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 described clearly and completely below. 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 creative work are within the scope of protection of this application.

[0030] Example 1

[0031] (1) Preparation of polishing liquid: weigh 1000 g of 300 μm cerium oxide powder and 16 g of zirconium oxychloride octahydrate (ZrOCl2·8H2O) powder, add deionized water, mix and dilute to 500 mL;

[0032] (2) Preparation of fluoride glass preform: The fluoride glass composition is 25.5InF3-18BaF2-8SrF2-15ZnF2-11.5GaF3-12NaF-5LiF-5YF3 in molar ratio. It is melted at 900°C for 2 hours in a CF4 atmosphere and poured into a mold to make a fluoride glass preform;

[0033] (3) Fluoride glass preform processing: After rough grinding and fine grinding of the fluoride glass preform, the fluoride glass preform is polished using a prepared polishing liquid;

[0034] (4) Drawing a fluoride glass preform: Using a drawing tower, the polished fluoride glass preform is drawn into a fluoride optical fiber.

[0035] Example 2

[0036] (1) Preparation of polishing liquid: weigh 1000 g of 300 μm cerium oxide powder and 16 g of zirconium oxychloride octahydrate (ZrOCl2·8H2O) powder, add deionized water, mix and dilute to 500 mL;

[0037] (2) Preparation of fluoride glass preform: The fluoride glass composition is 25.5InF3-18BaF2-8SrF2-15ZnF2-11.5GaF3-7NaF-5LiF-5YF3-5PbF2 in molar ratio. It is melted at 900°C for 2 hours in a CF4 atmosphere and poured into a mold to make a fluoride glass preform.

[0038] (3) Fluoride glass preform processing: After rough grinding and fine grinding of the fluoride glass preform, the fluoride glass preform is polished using a prepared polishing liquid;

[0039] (4) Drawing a fluoride glass preform: Using a drawing tower, the polished fluoride glass preform is drawn into a fluoride optical fiber.

[0040] Example 3

[0041] (1) Preparation of polishing liquid: weigh 1000 g of 300 μm cerium oxide powder and 16 g of zirconium oxychloride octahydrate (ZrOCl2·8H2O) powder, add deionized water, mix and dilute to 500 mL;

[0042] (2) Preparation of fluoride glass preform: The fluoride glass composition is 53ZrF4-20BaF2-4LaF3-3AlF3-2NaF3 in molar ratio. It is melted at 900°C for 2 hours in a CF4 atmosphere and poured into a mold to make a fluoride glass preform.

[0043] (3) Fluoride glass preform processing: After rough grinding and fine grinding of the fluoride glass preform, the fluoride glass preform is polished using a prepared polishing liquid;

[0044] (4) Drawing a fluoride glass preform: Using a drawing tower, the polished fluoride glass preform is drawn into a fluoride optical fiber.

[0045] Example 4

[0046] (1) Preparation of polishing liquid: weigh 1000 g of 300 μm cerium oxide powder and 16 g of zirconium oxychloride octahydrate (ZrOCl2·8H2O) powder, add deionized water, mix and dilute to 500 mL;

[0047] (2) Preparation of fluoride glass preform: The fluoride glass composition is 53ZrF4-17BaF2-4LaF3-3AlF3-2NaF3-3PbF2 in molar ratio. It is melted at 900°C for 2 hours in a CF4 atmosphere and poured into a mold to make a fluoride glass preform.

[0048] (3) Fluoride glass preform processing: After rough grinding and fine grinding of the fluoride glass preform, the fluoride glass preform is polished using a prepared polishing liquid;

[0049] (4) Drawing a fluoride glass preform: Using a drawing tower, the polished fluoride glass preform is drawn into a fluoride optical fiber.

[0050] Example 5

[0051] (1) Preparation of polishing liquid: weigh 500 g of 300 μm cerium oxide powder and 16 g of zirconium oxychloride octahydrate (ZrOCl2·8H2O) powder, add deionized water, mix and dilute to 500 mL;

[0052] (2) Preparation of fluoride glass preform: The fluoride glass composition is 25.5InF3-18BaF2-8SrF2-15ZnF2-11.5GaF3-12NaF-5LiF-5YF3 in molar ratio. It is melted at 900°C for 2 hours in a CF4 atmosphere and poured into a mold to make a fluoride glass preform;

[0053] (3) Fluoride glass preform processing: After rough grinding and fine grinding of the fluoride glass preform, the fluoride glass preform is polished using a prepared polishing liquid;

[0054] (4) Drawing a fluoride glass preform: Using a drawing tower, the polished fluoride glass preform is drawn into a fluoride optical fiber.

[0055] Example 6

[0056] (1) Preparation of polishing liquid: weigh 1500 g of 300 μm cerium oxide powder and 16 g of zirconium oxychloride octahydrate (ZrOCl2·8H2O) powder, add deionized water, mix and dilute to 500 mL;

[0057] (2) Preparation of fluoride glass preform: The fluoride glass composition is 53ZrF4-17BaF2-4LaF3-3AlF3-2NaF3-3PbF2 in molar ratio. It is melted at 900°C for 2 hours in a CF4 atmosphere and poured into a mold to make a fluoride glass preform.

[0058] (3) Fluoride glass preform processing: After rough grinding and fine grinding of the fluoride glass preform, the fluoride glass preform is polished using a prepared polishing liquid;

[0059] (4) Drawing a fluoride glass preform: Using a drawing tower, the polished fluoride glass preform is drawn into a fluoride optical fiber.

[0060] Example 7

[0061] (1) Preparation of polishing liquid: weigh 1000 g of 300 μm cerium oxide powder and 160 g of zirconium oxychloride octahydrate (ZrOCl2·8H2O) powder, add deionized water, mix and dilute to 500 mL;

[0062] (2) Preparation of fluoride glass preform: The fluoride glass composition is 53ZrF4-17BaF2-4LaF3-3AlF3-2NaF3-3PbF2 in molar ratio. It is melted at 900°C for 2 hours in a CF4 atmosphere and poured into a mold to make a fluoride glass preform.

[0063] (3) Fluoride glass preform processing: After rough grinding and fine grinding of the fluoride glass preform, the fluoride glass preform is polished using a prepared polishing liquid;

[0064] (4) Drawing a fluoride glass preform: Using a drawing tower, the polished fluoride glass preform is drawn into a fluoride optical fiber.

[0065] Comparative Example 1

[0066] The other steps are the same as those in Example 1, except that zirconium oxychloride octahydrate (ZrOCl2·8H2O) is not added to the preparation of the polishing liquid.

[0067] Comparative Example 2

[0068] The other steps are the same as those in Example 2, except that zirconium oxychloride octahydrate (ZrOCl2·8H2O) is not added to the preparation of the polishing liquid.

[0069] Comparative Example 3

[0070] The other steps are the same as those in Example 3, except that zirconium oxychloride octahydrate (ZrOCl2·8H2O) is not added to the preparation of the polishing liquid.

[0071] Comparative Example 4

[0072] The other steps are the same as those in Example 4, except that zirconium oxychloride octahydrate (ZrOCl2·8H2O) is not added to the preparation of the polishing liquid.

[0073] The surface roughness of the fluoride glass preforms after polishing in the above seven embodiments and four comparative examples is shown in Table 1 below:

[0074] Table 1

[0075] Roughness(mm) Example 1 0.009 Example 2 0.011 Example 3 0.005 Example 4 0.008 Example 5 0.012 Example 6 0.007 Example 7 0.005 Comparative Example 1 0.025 Comparative Example 2 0.027 Comparative Example 3 0.033 Comparative Example 4 0.021

[0076] It can be seen from Table 1 that, by adding an appropriate amount of zirconium oxychloride to a conventional polishing liquid (prepared from cerium oxide and water), the generation of fluoride on the surface of the fluoride glass can be reduced, and the surface roughness of the fluoride glass can be reduced.

[0077] The losses of the fluoride optical fibers drawn from the fluoride glass preforms in the above seven embodiments and four comparative examples are shown in Table 2 below:

[0078] Table 2

[0079]

[0080]

[0081] It can be seen from Table 2 that by adding an appropriate amount of zirconium dichloride to a conventional polishing liquid (prepared with cerium oxide and water), the generation of fluoride on the surface of fluoride glass can be reduced, thereby reducing the optical fiber loss.

[0082] In summary, the present invention discloses a special polishing liquid for fluoride glass, and its preparation method and application. The composition of the polishing liquid is water (H2O), cerium oxide (CeO2) and zirconium oxychloride (ZrOCl2). The preparation method of the polishing liquid comprises the following steps: step 1, weighing 500-1500 grams of 300 micron cerium oxide and 16-160 grams of zirconium oxychloride octahydrate (ZrOCl2·8H2O); step 2, adding deionized water to the weighed cerium oxide and zirconium oxychloride octahydrate, mixing, and fixing the volume to 500mL; step 3, using the above-prepared polishing liquid for surface polishing of fluoride special laser glass. The product of the present invention is not only simple to prepare and green and environmentally friendly, but also can effectively reduce the crystallization phenomenon on the surface of fluoride glass and reduce optical fiber loss when applied to fluoride glass polishing.

[0083] 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 special polishing liquid for fluoride glass, characterized in that: The polishing liquid comprises cerium oxide, zirconium oxychloride and water. The concentration of the cerium oxide is 1-5 g / mL, and the concentration of the zirconium oxychloride is 0.1-1 mol / L.

2. The fluoride glass-specific polishing liquid according to claim 1, characterized in that: Each 500 mL of the polishing liquid is prepared by adding 500 to 2500 grams of cerium oxide powder and 16 to 160 grams of zirconium oxychloride octahydrate powder into deionized water and mixing.

3. The special polishing liquid for fluoride glass according to claim 2, characterized in that: The particle size of the cerium oxide powder is 100-300 nanometers.

4. A method for preparing a special polishing liquid for fluoride glass, characterized in that: The method comprises the following steps: mixing cerium oxide, zirconium oxychloride and water to obtain a polishing liquid; wherein the concentration of the cerium oxide is 1-5 g / mL, and the concentration of the zirconium oxychloride is 0.1-1 mol / L.

5. The method for preparing a special polishing liquid for fluoride glass according to claim 4, characterized in that: The specific steps include: Step 1, weighing 500-2500 g of cerium oxide powder and 16-160 g of zirconium oxychloride octahydrate powder; Step 2: add deionized water to the weighed cerium oxide powder and zirconium oxychloride octahydrate powder, mix, and dilute to 500 mL to obtain the polishing liquid.

6. The method for preparing the special polishing liquid for fluoride glass according to claim 5, characterized in that: The particle size of the cerium oxide powder is 100-300 nanometers.

7. A special polishing liquid for fluoride glass according to any one of claims 1 to 3, used for polishing fluoride glass.

8. The use according to claim 7, characterized in that: The composition of the fluoride glass includes InF3, BaF2, SrF2, ZnF2, GaF3, NaF, LiF and YF3; Alternatively, the composition of the fluoride glass includes InF3, BaF2, SrF2, ZnF2, GaF3, NaF, LiF, YF3 and PbF2; Alternatively, the composition of the fluoride glass includes ZrF4, BaF2, LaF3, AlF3 and NaF; Alternatively, the composition of the fluoride glass includes ZrF4, BaF2, LaF3, AlF3, NaF and PbF2.

9. The use according to claim 7, characterized in that: The method of application comprises the steps of: Fluoride glass is available; Making the fluoride glass into a fluoride glass preform; After rough grinding and fine grinding of the fluoride glass preform, the fluoride glass preform is polished using the polishing liquid; The polished fluoride glass preform is drawn into a fluoride optical fiber using a drawing tower.

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