A method for mass production of infrared chalcogenide glass microspheres
By using a multi-core optical fiber heat treatment method, the problem of low preparation efficiency of chalcogenide glass microspheres has been solved, and efficient and low-cost mass production has been achieved. The prepared microspheres have broad application prospects in the infrared field.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-03-01
- Publication Date
- 2026-03-13
AI Technical Summary
The existing technology for preparing chalcogenide glass microspheres has low efficiency and makes it difficult to achieve low-cost, large-scale preparation.
A multi-core optical fiber heat treatment method is adopted, which involves preparing multi-core optical fibers and heat-treating them by tightly packing them together. This reduces the amount of thermoplastic polymer cladding used, thereby improving preparation efficiency and reducing costs.
It significantly improves the preparation efficiency of chalcogenide glass microspheres, with a single preparation yield of up to one million microspheres, reducing costs. Furthermore, the prepared microspheres have uniform diameter, low eccentricity, and high quality factor, making them suitable for applications such as infrared retroreflection, microcavity sensing, and nonlinear optics.
Smart Images

Figure CN118084307B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to a method for preparing glass microspheres, specifically a method for the batch preparation of infrared chalcogenide glass microspheres. Background Technology
[0002] Glass microspheres are a high-performance reflective material (also known as retroreflective material) that has been widely used in road safety, building decoration, aerospace, and other fields. Glass microspheres also serve as a high-performance optical resonator, characterized by high quality factor, small mode volume, narrow resonant mode width, and high intracavity energy density. They hold great potential for applications in high-sensitivity sensors, narrowband filters, low-threshold lasers, and nonlinear optics. In recent years, with advancements in infrared technology, the demand for infrared glass microspheres operating within atmospheric high-transparency windows of 3–5 μm and 8–12 μm has been increasing. For example, aerospace equipment requires large quantities of glass microspheres with diameters of 50–300 μm as infrared reflective materials.
[0003] Chalcogenide glasses (amorphous materials formed based on chalcogen elements S, Se, and Te) are the only glass materials whose light transmission range can cover the 3–5 μm and 8–12 μm wavelength bands. Furthermore, chalcogenide glasses possess high refractive index, excellent chemical stability, and superior thermal stability, making chalcogenide glass microspheres considered excellent infrared reflective materials. Currently, there are three main methods for preparing chalcogenide glass microspheres. The first method is the "high-temperature molten powder method," where chalcogenide glass powder is poured into a tube furnace with a protective atmosphere. The powder is heated and forms spheres due to surface tension as it falls through the furnace. Using this method, the chalcogenide glass powder undergoes significant volatilization upon heating, resulting in a low sphere formation rate; the material utilization rate from glass crushing and sieving to final sphere formation is typically <10%. The second method is the "fiber fusion sphere method," which uses a laser or ring heater to heat the fine end of an optical fiber to obtain microspheres. Microspheres prepared using this method have extremely high quality factors, but typically only a few microspheres can be prepared at a time, resulting in very low preparation efficiency. The third method is the "fiber fusion method" (ZL201310593026.7), which involves heating a chalcogenide glass / polymer composite optical fiber to near its softening temperature, causing the chalcogenide glass filaments inside the polymer to break and form microspheres. This method can produce a large number of microspheres in a single operation, with a material utilization rate typically exceeding 30%, and the microspheres have a high quality factor. However, forming microspheres requires the use of thick polymer-clad optical fibers to achieve good confinement of the fiber core at high temperatures. This consumes a large amount of expensive polymer and organic solvents for dissolving the polymer, making it difficult to achieve low-cost, large-scale production of chalcogenide glass microspheres. Summary of the Invention
[0004] To address the problems of low preparation efficiency and difficulty in achieving low-cost mass production of chalcogenide glass microspheres in existing technologies, this invention provides a method for mass production of infrared chalcogenide glass microspheres by stacking multi-core optical fibers with thin polymer cladding and performing heat treatment, which significantly improves the preparation efficiency and reduces the preparation cost of glass microspheres.
[0005] To address the problems of the existing technology, the technical solution adopted by the present invention is as follows:
[0006] A method for mass production of infrared chalcogenide glass microspheres includes the following steps:
[0007] (1) Fabrication of multi-core optical fibers
[0008] A chalcogenide glass rod with a diameter of d1 is prepared in a vacuum quartz tube using a melt-quench method. This rod is then inserted into a thermoplastic polymer sleeve with inner and outer diameters of d1 and d2, respectively, to form a first optical fiber preform, where d2 / d1 = 1.4–2.0. The first optical fiber preform is then drawn into a thin rod with a diameter of d3. Several thin rods are tightly packed into a hollow cuboid metal mold, and the tightly packed rods are then heat-treated to bond the thermoplastic polymer on their surfaces together, forming a second optical fiber preform. The second optical fiber preform is then drawn into a multi-core optical fiber with a diagonal length of d4.
[0009] (2) Preparation of chalcogenide glass microspheres by heat treatment of multi-core optical fibers
[0010] Several multi-core optical fibers prepared in step (1) are tightly stacked into a hollow cuboid metal mold. Then, the two ends of the mold are blocked and placed in a vacuum furnace. The vacuum degree inside the furnace is evacuated to <1 kPa. Then, the furnace temperature is raised to 300-360℃ for heat treatment for 10-30 minutes to break the glass core in the multi-core optical fiber and form glass microspheres.
[0011] (3) The polymer was washed and sieved to obtain uniformly sized chalcogenide glass microspheres.
[0012] Remove the heat-treated multi-core optical fiber from the metal mold in step (2) and place it in a beaker containing organic solvent and magnetic stirrer. Place the beaker on the heating platform of a magnetic stirrer and set the heating platform temperature so that the thermoplastic polymer dissolves rapidly into the organic solvent with stirring and heating. Replace the organic solvent every 30 to 60 minutes, and repeat 3 to 5 times to ensure that the thermoplastic polymer is completely dissolved. Rinse the glass microspheres in the beaker with anhydrous ethanol 3 to 5 times, and then sieve the glass microspheres and anhydrous ethanol together to obtain glass microspheres with uniform size. Finally, dry the glass microspheres.
[0013] Preferably, the glass transition temperature of the chalcogenide glass rod in step (1) is 160℃~200℃.
[0014] Preferably, the thermoplastic polymer sleeve in step (1) is made of polyetherimide (PEI), polyethersulfone (PES), or polysulfone (PSU).
[0015] Preferably, the diameter d3 in step (1) is 1.5 to 3 mm; d4 is greater than 800 μm.
[0016] Preferably, the diameter of the glass microspheres in step (2) is 60 to 300 μm.
[0017] Preferably, the organic solvent in step (3) is dimethylacetamide, and the temperature of the heating platform is set to 50°C to 60°C.
[0018] Beneficial effects:
[0019] Compared with existing technologies, the present invention provides a method for the mass production of infrared chalcogenide glass microspheres, which has the following advantages:
[0020] (1) This invention prepares chalcogenide glass microspheres by “preparing multi-core optical fibers and then tightly stacking multiple multi-core optical fibers and performing heat treatment”. By increasing the number of cores in the multi-core optical fibers and the number of stacked multi-core optical fibers, the preparation efficiency can be greatly improved, and the number of microspheres prepared in a single batch can reach more than one million.
[0021] (2) In the preparation method of this invention, the close stacking of multi-core optical fibers promotes mutual binding between the fibers. Even with a thinner thermoplastic polymer cladding, sufficient binding can be achieved to ensure the formation of microspheres during heat treatment. Compared with existing methods for preparing microspheres from heat-treated optical fibers, the ratio of the thermoplastic polymer cladding diameter to the fiber core diameter (=d2 / d1) of this invention is reduced from ≥3 to 1.4~2.0, the amount of polymer used is reduced by more than half, and the amount of organic solvent used to dissolve the polymer is also reduced by more than half, which can significantly reduce costs.
[0022] (3) Using this invention, microcavities with diameters of 60–300 μm, eccentricity <2%, and quality factor Q ≥ 2x10 can be prepared. 5 Chalcogenide glass microspheres have great application prospects in fields such as infrared retroreflection, microcavity sensing, infrared laser generation, and nonlinear optics. Attached Figure Description
[0023] Figure 1 This is a schematic diagram of the fabrication of the first optical fiber preform (left), the fabrication of the second optical fiber preform (middle), and the close stacking of multi-core optical fibers (right) in Example 1;
[0024] Figure 2 This is an optical photograph of the chalcogenide glass microspheres prepared in Example 1;
[0025] Figure 3Optical photographs of the chalcogenide glass microspheres prepared in Comparative Example 1;
[0026] Figure 4 This is an optical photograph of the chalcogenide glass microspheres prepared in Comparative Example 2. Detailed Implementation
[0027] The following embodiments further illustrate the content of the present invention, but should not be construed as limiting the present invention. Modifications and substitutions made to the methods, steps, or conditions of the present invention without departing from the spirit and essence of the invention are all within the scope of the present invention. Unless otherwise specified, the technical means used in the embodiments are conventional means well known to those skilled in the art.
[0028] Example 1
[0029] A method for batch preparation of infrared chalcogenide glass microspheres, wherein the chemical formula of the chalcogenide glass microspheres prepared in this embodiment is Ge. 10 As 30 Se 40 Te 20 The glass has a glass transition temperature of 170℃. The specific preparation method is as follows: using elemental Ge, As, Se, and Te with a purity ≥99.999% as raw materials, a Ge glass with a diameter of 15mm and a length of 150mm is prepared in a vacuum quartz tube using a melt-quench method. 10 As 30 Se 40 Te 20 A chalcogenide glass rod (weighing approximately 130g) is inserted into a polyetherimide (PEI) sleeve with inner and outer diameters of 15mm and 24mm respectively to form the first optical fiber preform. Figure 1 As shown in the left-middle figure; the first optical fiber preform is drawn into a thin rod with a diameter of 2 mm; 60 thin rods with a length of approximately 280 mm are tightly packed into a hollow cuboid metal mold, and then the tightly packed thin rods are heat-treated to bond the PEI on their surfaces together, forming a second optical fiber preform with dimensions of approximately 16 mm x 14.1 mm x 280 mm, as shown in the figure below. Figure 1 As shown in the middle figure; the second optical fiber preform is drawn into a multi-core optical fiber with a diagonal length of approximately 850 μm, corresponding to a single core diameter of approximately 50 μm; 900 multi-core optical fibers, each approximately 175 mm in length, are tightly packed into a hollow cuboid metal mold, as shown. Figure 1As shown in the middle right figure, the two ends of the mold are then blocked. The mold containing the multi-core optical fiber is placed in a vacuum furnace, and a vacuum is drawn to a vacuum level of <1 kPa. The furnace temperature is then raised to 340℃ for heat treatment for 20 minutes, causing the glass core in the multi-core optical fiber to break and form glass microspheres. The heat-treated multi-core optical fiber is removed from the metal mold and placed in a beaker containing dimethylacetamide and a magnetic stirrer. The beaker is then placed on the heating platform of a magnetic stirrer, and the heating platform temperature is set to 50℃, allowing PEI to dissolve quickly into the organic solvent with stirring and heating. The organic solvent is replaced every 60 minutes, for a total of 3 times, to ensure complete dissolution of PEI. The glass microspheres in the beaker are rinsed 5 times with anhydrous ethanol. The glass microspheres and anhydrous ethanol are then passed through 80-mesh and 100-mesh sieves to obtain glass microspheres of uniform size. Finally, the glass microspheres are dried.
[0030] The size and eccentricity of the glass microspheres were measured using a size-calibrated optical microscope, the weight of the glass microspheres was weighed using an electronic balance with an accuracy of 0.01 g, and the microcavity quality factor Q was measured using a tapered fiber optic coupling measurement system.
[0031] The test results showed that over 80% of the obtained glass microspheres had a diameter of 160–180 μm, and the eccentricity of these microspheres was <2%. Figure 2 As shown; the weight of the glass microspheres is approximately 51.48g, containing approximately 3.7 x 10⁻⁶ microspheres. 6 Each glass microsphere; microcavity quality factor Q = 4 x 10⁻⁶ 5 (@8.3μm).
[0032] Example 2
[0033] A method for batch preparation of infrared chalcogenide glass microspheres, wherein the chemical formula of the chalcogenide glass microspheres prepared in this embodiment is As. 40 S 60 The glass has a glass transition temperature of 200℃. The specific preparation method is as follows: using elemental As and S with a purity ≥99.999% as raw materials, an As glass with a diameter of 15mm and a length of 150mm is prepared in a vacuum quartz tube using a melt-quench method. 40 S 60A chalcogenide glass rod (weighing approximately 84.6 g) is inserted into a polyethersulfone (PES) sleeve with inner and outer diameters of 15 mm and 30 mm, respectively, to form a first optical fiber preform. The first optical fiber preform is drawn into a thin rod with a diameter of 1.5 mm. 189 thin rods, each approximately 250 mm long, are tightly packed into a hollow cuboid metal mold. The tightly packed rods are then heat-treated to bond the PES on their surfaces together, forming a shape approximately 21 mm x 18.4 mm x 18.4 mm. A 250mm second optical fiber preform is used; this preform is drawn into a multi-core optical fiber with a diagonal length of approximately 930μm, corresponding to a single core diameter of approximately 25μm; 900 multi-core optical fibers, each approximately 225mm long, are tightly packed into a hollow cuboid metal mold, and then the two ends of the mold are sealed; the mold containing the multi-core optical fibers is placed in a vacuum furnace, and a vacuum level of <1kPa is created. The furnace temperature is then raised to 360℃ for heat treatment for 30 minutes, causing the glass cores in the multi-core optical fibers to break and form glass microspheres; the heat-treated multi-core optical fibers are then... The optical fiber core is removed from the metal mold and placed in a beaker containing dimethylacetamide and a magnetic stirrer. The beaker is then placed on the heating platform of a magnetic stirrer, and the heating platform temperature is set to 60°C to allow the PES to dissolve quickly into the organic solvent through stirring and heating. The organic solvent is replaced every 30 minutes, for a total of 5 replacements, to ensure complete dissolution of the PES. The glass microspheres in the beaker are rinsed 3 times with anhydrous ethanol. The glass microspheres and anhydrous ethanol are then passed through 200-mesh and 230-mesh sieves to obtain glass microspheres of uniform size. Finally, the glass microspheres are dried.
[0034] The size and eccentricity of the glass microspheres were measured using a size-calibrated optical microscope, the weight of the glass microspheres was weighed using an electronic balance with an accuracy of 0.01 g, and the microcavity quality factor Q was measured using a tapered fiber optic coupling measurement system.
[0035] The test results showed that over 80% of the obtained glass microspheres had a diameter of 60–70 μm, and the eccentricity of these microspheres was <2%; the weight of the glass microspheres was approximately 32.32 g, containing approximately 7.0 x 10⁻⁶ microspheres. 7 Each glass microsphere; microcavity quality factor Q = 2 x 10⁻⁶ 5 (@4.6μm).
[0036] Example 3
[0037] A method for batch preparation of infrared chalcogenide glass microspheres, wherein the chemical formula of the chalcogenide glass microspheres prepared in this embodiment is As. 37 Se 63 The glass has a glass transition temperature of 160℃. The specific preparation method is as follows: using elemental As and Se with a purity ≥99.999% as raw materials, an As glass with a diameter of 15mm and a length of 150mm is prepared in a vacuum quartz tube using a melt-quench method.37 Se 63 A chalcogenide glass rod (weighing approximately 122g) is inserted into a polysulfone (PSU) sleeve with inner and outer diameters of 15mm and 21mm respectively to form a first optical fiber preform. The first optical fiber preform is then drawn into a thin rod with a diameter of 3mm. Thirty-nine thin rods, each approximately 150mm in length, are tightly packed into a hollow cuboid metal mold. The tightly packed rods are then heat-treated to bond the PSU on their surfaces together, forming a shape approximately 18mm x 18.6mm x A 150mm second optical fiber preform is used; this preform is drawn into a multi-core optical fiber with a diagonal length of approximately 1200μm, corresponding to a single core diameter of approximately 100μm; 440 multi-core optical fibers, each approximately 140mm long, are tightly packed into a hollow cuboid metal mold, and then the two ends of the mold are sealed; the mold containing the multi-core optical fibers is placed in a vacuum furnace, and a vacuum level of <1kPa is created. The furnace temperature is then raised to 300℃ for heat treatment for 10 minutes, causing the glass cores in the multi-core optical fibers to break and form glass microspheres; the heat-treated... The multi-core optical fiber was removed from the metal mold and placed in a beaker containing dimethylacetamide and a magnetic stirrer. The beaker was then placed on the heating platform of a magnetic stirrer, and the heating platform temperature was set to 55°C to allow the PSU to dissolve quickly into the organic solvent with stirring and heating. The organic solvent was replaced every 45 minutes, for a total of 4 replacements, to ensure complete dissolution of the PSU. The glass microspheres in the beaker were rinsed 4 times with anhydrous ethanol. Then, the glass microspheres and anhydrous ethanol were passed through 50-mesh and 60-mesh sieves to obtain glass microspheres of uniform size. Finally, the glass microspheres were dried.
[0038] The size and eccentricity of the glass microspheres were measured using a size-calibrated optical microscope, the weight of the glass microspheres was weighed using an electronic balance with an accuracy of 0.01 g, and the microcavity quality factor Q was measured using a tapered fiber optic coupling measurement system.
[0039] The test results showed that over 80% of the obtained glass microspheres had a diameter of 270–300 μm, and the eccentricity of these microspheres was <2%; the weight of the glass microspheres was approximately 50.95 g, containing approximately 1.1 x 10⁻⁶ microspheres. 6 Each glass microsphere; microcavity quality factor Q = 6 x 10⁻⁶ 5 (@4.6μm).
[0040] Comparative Example 1
[0041] The chemical formula of the chalcogenide glass microspheres prepared in this comparative example is Ge. 10 As 30 Se 40 Te 20The glass has a glass transition temperature of 170℃. The main difference between its preparation method and Example 1 is that d2 / d1 < 1.4. The specific preparation method is as follows: using elemental Ge, As, Se, and Te with a purity ≥ 99.999% as raw materials, a Ge glass with a diameter of 15mm and a length of 150mm is prepared in a vacuum quartz tube using a melt-quench method. 10 As 30 Se 40 Te 20 A chalcogenide glass rod (weighing approximately 130g) is inserted into a PEI sleeve with inner and outer diameters of 15mm and 19.5mm respectively to form a first optical fiber preform. The first optical fiber preform is drawn into a thin rod with a diameter of 1.63mm. Sixty thin rods, each approximately 280mm long, are tightly packed into a hollow cuboid metal mold. The tightly packed rods are then heat-treated to bond the PEI on their surfaces together, forming an optical fiber with dimensions of approximately 13mm x 11.5mm x 19.5mm. A 280mm second optical fiber preform is used; this preform is drawn into a multi-core optical fiber with a diagonal length of approximately 700μm, corresponding to a single core diameter of approximately 50μm; 900 multi-core optical fibers, each approximately 175mm in length, are tightly packed into a hollow cuboid metal mold, and then the two ends of the mold are sealed; the mold containing the multi-core optical fibers is placed in a vacuum furnace, and a vacuum is drawn to a level <1kPa. The furnace temperature is then raised to 340℃ for heat treatment for 20 minutes, causing the glass core in the multi-core optical fiber to fracture and form glass microfibers. The heat-treated multi-core optical fiber was removed from the metal mold and placed in a beaker containing dimethylacetamide and a magnetic stirrer. The beaker was then placed on the heating platform of a magnetic stirrer, and the heating platform temperature was set to 50°C, allowing the PEI to dissolve quickly into the organic solvent with stirring and heating. The organic solvent was replaced every 60 minutes, for a total of 3 times, to ensure complete dissolution of the PEI. The glass microspheres in the beaker were rinsed 5 times with anhydrous ethanol, and then the glass microspheres and anhydrous ethanol were passed through 80-mesh and 100-mesh sieves. Finally, the glass microspheres were dried.
[0042] Observation of glass microspheres using a size-calibrated optical microscope revealed that many multi-core optical fibers, after their glass cores broke, were difficult to form microspheres, resulting in a very low sphericity rate. Figure 3 As shown.
[0043] The results of Comparative Example 1 show that it is difficult to form microspheres and the sphere formation rate is very low. This is related to the excessively thin polymer coating. During heat treatment, the thin polymer cannot provide sufficient binding to the fractured and deformed fiber core to form microspheres.
[0044] Comparative Example 2
[0045] The chemical formula of the chalcogenide glass microspheres prepared in this comparative example is Ge. 10 As 30 Se40 Te 20 The glass has a glass transition temperature of 170℃. The main difference between its preparation method and Example 1 is that the multi-core optical fibers are not tightly packed; instead, several multi-core optical fibers are randomly placed into a vacuum furnace for heat treatment. The specific preparation method is as follows: using elemental Ge, As, Se, and Te with a purity ≥99.999% as raw materials, a Ge fiber with a diameter of 15mm and a length of 150mm is prepared in a vacuum quartz tube using a melt-quench method. 10 As 30 Se 40 Te 20 A chalcogenide glass rod (weighing approximately 130g) is inserted into a PEI sleeve with inner and outer diameters of 15mm and 24mm respectively to form a first optical fiber preform. The first optical fiber preform is then drawn into a thin rod with a diameter of 2mm. Sixty thin rods, each approximately 280mm long, are tightly packed into a hollow cuboid metal mold. The tightly packed rods are then heat-treated to bond the PEI on their surfaces together, forming a shape approximately 16mm x 14.1mm x A 280mm second optical fiber preform was used. This preform was drawn into a multi-core optical fiber with a diagonal length of approximately 850μm, corresponding to a single core diameter of approximately 50μm. 900 multi-core optical fibers, each approximately 175mm long, were randomly placed in a metal tray. The tray was then placed in a vacuum furnace, and a vacuum level of <1kPa was created. The furnace temperature was then raised to 340℃ for heat treatment for 20 minutes, causing the glass cores of the multi-core optical fibers to break and form glass microspheres. The heat-treated multi-core optical fibers were removed from the metal tray and placed in a beaker containing dimethylacetamide and a magnetic stirrer. The beaker was then placed on the heating platform of a magnetic stirrer, with the platform temperature set to 50℃, allowing the PEI to dissolve rapidly in the organic solvent with stirring and heating. The organic solvent was replaced every 60 minutes for a total of three times to ensure complete dissolution of the PEI. The glass microspheres in the beaker were rinsed five times with anhydrous ethanol, and finally dried.
[0046] Observation of the glass microspheres using a size-calibrated optical microscope revealed that the obtained glass microspheres were highly non-uniform in size (150–500 μm), and a large number of microspheres were elliptical in shape, such as… Figure 4 As shown.
[0047] The results of Comparative Example 2 show that the glass microspheres are not uniform in size, and a large number of microspheres are elliptical. This is related to the binding state of the polymer on the glass fiber core during heat treatment. When the multi-core optical fibers are arranged randomly, a uniform binding cannot be formed between neighboring multi-core optical fibers, resulting in very uneven glass microsphere sizes.
[0048] In summary, this invention prepares chalcogenide glass microspheres by "preparing multi-core optical fibers, then tightly stacking multiple multi-core optical fibers and performing heat treatment." Increasing the number of cores in the multi-core optical fibers and the number of stacked multi-core optical fibers significantly improves the preparation efficiency, allowing for the production of over one million microspheres in a single batch. The prepared chalcogenide glass microspheres have a diameter of 60–300 μm, an eccentricity of <2%, and a microcavity quality factor Q ≥ 2 x 10⁻⁶. 5 It has great application prospects in fields such as infrared retroreflection, microcavity sensing, infrared laser generation, and nonlinear optics.
[0049] The present invention and its embodiments have been described above illustratively. This description is not restrictive, and the figures shown are only one embodiment of the present invention; the actual structure is not limited thereto. Therefore, if those skilled in the art are inspired by this description and design similar structures and embodiments without departing from the spirit of the present invention, such designs should fall within the protection scope of the present invention.
Claims
1. A method for batch production of infrared chalcogenide glass microbeads, characterized in that, The method comprises the following steps: (1) preparing a multicore optical fiber A rod of chalcogenide glass with a diameter of d1 is prepared by a melt-quenching method in a vacuum quartz tube, and the rod is inserted into a thermoplastic polymer sleeve with an inner diameter of d1 and an outer diameter of d2 to form a first optical fiber preform, wherein d2 / d1 = 1.4-2.0; the first optical fiber preform is drawn into a thin rod with a diameter of d3; a plurality of thin rods are tightly packed into a hollow cuboid metal mold, and then the tightly packed thin rods are heat treated to make the thermoplastic polymer on the surface of the thin rods adhere together to form a second optical fiber preform; the second optical fiber preform is drawn into a multicore optical fiber with a diagonal length of d4; (2) heat treating the multicore optical fiber to prepare chalcogenide glass microbeads A plurality of the multicore optical fibers prepared in step (1) are tightly packed into a hollow cuboid metal mold, then the two ports of the mold are blocked, placed in a vacuum furnace, vacuum is drawn to make the vacuum degree in the furnace <1 kPa, then the furnace temperature is raised to 300~360 o C is heated for 10~30 minutes to make the glass cores in the multicore optical fibers break to form glass microbeads; (3) cleaning the polymer and sieving to obtain chalcogenide glass microbeads with uniform size The multicore optical fiber after heat treatment in step (2) is taken out of the metal mold, placed in a beaker containing an organic solvent and a magnet, and the beaker is placed on the heating platform of a magnetic stirrer, and the temperature of the heating platform is set so that the thermoplastic polymer is quickly dissolved into the organic solvent with stirring and heating; the organic solvent is replaced every 30-60 minutes, and the replacement is continuously performed 3-5 times to completely dissolve the thermoplastic polymer; the glass microbeads in the beaker are then rinsed with anhydrous ethanol for 3-5 times, and the glass microbeads and anhydrous ethanol are sieved together to obtain glass microbeads with uniform size; finally, the glass microbeads are dried.
2. The method of claim 1, wherein the infrared chalcogenide glass microbeads are prepared in a batch process. The glass transition temperature of the chalcogenide glass rod in step (1) is 160 o C~200 o C.
3. The method of claim 1, wherein the infrared chalcogenide glass microbeads are prepared in a batch process. The material of the thermoplastic polymer sleeve in step (1) is polyetherimide, polyether sulfone or polysulfone.
4. The method of claim 1, wherein the infrared chalcogenide glass microbeads are prepared in bulk. In step (1), the diameter d3 = 1.5-3 mm; d4 > 800 μm.
5. The method of claim 1, wherein the infrared chalcogenide glass microbeads are prepared in bulk. In step (2), the diameter of the glass microbeads is 60-300 μm.
6. The method of claim 1, wherein the infrared chalcogenide glass microbeads are prepared in bulk. The organic solvent in step (3) is dimethylacetamide; the temperature of the heating platform is set to 50 o C60 o C.
Citation Information
Patent Citations
A method for preparing high-performance chalcogenide glass microspheres
CN103613276B
High-performance chalcogenide glass microsphere and preparation method thereof
CN103613276A
Preparation method of chalcogenide glass microspheres
CN112745030A