Submicron-diameter ice micro-nano optical fiber and preparation device and method thereof

By employing a photothermal-induced refined processing method, and utilizing an infrared light source and a quartz fiber taper to locally sublimate initial ice micro/nano fibers, submicron diameter ice micro/nano fibers with controllable diameters were successfully fabricated. This solved the fabrication challenges in existing technologies and achieved high-quality fiber fabrication.

CN121578437APending Publication Date: 2026-02-27ZHEJIANG UNIV
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Patent Information

Application Number
CN202511798540.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-12-02
Publication Date
2026-02-27

AI Technical Summary

Technical Problem

Existing technologies are insufficient for the stable fabrication of submicron diameter ice micro/nano fibers with controllable diameter and reliable quality, which limits the development of ice-based photonic devices in strong light field manipulation and extreme application scenarios.

Method used

By employing a photothermal-induced fine processing strategy, the initial ice micro/nano fiber was locally sublimated using an infrared light source and a quartz fiber taper, achieving controllable reduction in diameter and fabricating high-quality submicron diameter ice micro/nano fibers ranging from 10 to 500 nanometers.

Benefits of technology

Stable fabrication of submicron diameter ice micro/nano optical fibers has been achieved, with smooth surfaces, good diameter uniformity, excellent mechanical properties, and low-loss single-mode optical waveguide characteristics, thus solving the technical bottleneck of traditional methods.

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Abstract

The invention discloses a submicron-diameter ice micro-nano optical fiber and a preparation device and method thereof. The initial ice micro-nano optical fiber is clamped and fixed by an optical fiber clamping object and is in a suspended state; the infrared light source is connected with the silica optical fiber taper, and the silica optical fiber taper is arranged in the direction perpendicular to the axial direction of the initial ice micro-nano optical fiber and conducts scanning movement in the axial direction; based on the strong absorption characteristic of ice in an infrared band, infrared light energy is conducted through a quartz optical fiber taper, light intensity and scanning speed are regulated and controlled, local heating of a specific area of an initial ice micro-nano optical fiber is achieved, the ice micro-nano optical fiber is promoted to generate a controllable gasification sublimation process, and therefore the ice optical fiber is manufactured by reducing the diameter of the ice optical fiber to the submicron scale. The method is simple in process and high in regulation and control precision, the submicron-diameter ice micro-nanofiber which is difficult to implement in the past can be stably prepared, and the prepared submicron-diameter ice micro-nanofiber is smooth in surface, good in diameter uniformity and adjustable in diameter and uniform region length and has excellent mechanical performance and low-loss single-mode wave guiding capacity.
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Description

Technical Field

[0001] This invention relates to the field of micro-nano photonic materials preparation technology, and in particular to a submicron-scale ice fiber structure, specifically a submicron-diameter ice micro-nano fiber and its preparation device and method. Background Technology

[0002] Ice-based micro / nano fibers are a class of low-dimensional optical waveguides composed of water ice (H2O), exhibiting unique application potential in fields such as low-temperature photonics, high-sensitivity sensing, and transient optical devices. To meet the demands of these cutting-edge applications, ideal ice-based micro / nano fibers not only need a highly uniform structure and a smooth surface, but also require precisely tunable small diameters. Especially important are ice-based micro / nano fibers with submicron-scale diameters, which are crucial for achieving strong optical field confinement, enhancing nonlinear optical effects, and constructing miniaturized ice-based photonic functional devices.

[0003] Currently, electric field-enhanced assisted growth (EVL-AAG) is the mainstream technique for fabricating high-quality ice micro / nano fibers. While this method can achieve the initial formation of ice micro / nano fibers, its growth process relies on the random condensation and spontaneous growth of water molecules in an electric field, resulting in insufficient control over the final fiber diameter and high randomness. Consequently, the fabricated fibers mostly have diameters greater than 1 micrometer, while submicron ice micro / nano fibers with diameters less than 1 micrometer, especially those with uniform structures, are difficult to obtain consistently, constituting a significant technical bottleneck in this field.

[0004] In summary, current technologies lack an effective method for further refining grown ice micro / nano fibers to fabricate submicron diameter ice micro / nano fibers with controllable diameter and reliable quality. This technological gap significantly restricts the development of ice-based photonic devices in more demanding optical field manipulation and extreme application scenarios. Summary of the Invention

[0005] The present invention aims to address the deficiencies in the prior art by providing a submicron diameter ice micro / nano optical fiber and its fabrication apparatus and method.

[0006] This invention utilizes the strong absorption characteristics of ice materials in the infrared band and innovatively employs a photothermal-induced refined processing strategy. By locally and controlled sublimating the initial ice micro / nano fiber, its diameter can be controllably reduced. This method effectively overcomes the technical bottleneck of traditional electric field-enhanced assisted growth methods in fabricating submicron diameter ice fibers. It can stably fabricate high-quality submicron diameter ice micro / nano fibers with diameters ranging from 10 to 500 nanometers, providing a key material and technological foundation for the development of low-temperature photonics and ice-based nanophotonic devices.

[0007] To achieve the above objectives, the present invention adopts the following technical solution: I. A type of submicron diameter ice micro / nano optical fiber: The submicron diameter ice micro-nano fiber has a diameter of 10-500 nm and is prepared from initial ice micro-nano fiber through thermally induced sublimation.

[0008] II. An apparatus for fabricating the submicron diameter ice micro / nano optical fiber: The device includes an initial ice micro / nano fiber, a first fiber holder, a second fiber holder, an infrared light source, and a quartz fiber taper. The initial ice micro / nano fiber is clamped and fixed by the first and second fiber holders, with one end suspended. One end of the quartz fiber taper is connected to the infrared light source, which provides the light energy required for processing. The other end of the quartz fiber taper is fixed to a precision displacement stage, arranged perpendicular to the axis of the initial ice micro / nano fiber, and facing the suspended end of the initial ice micro / nano fiber.

[0009] The quartz fiber taper can be arranged in a scanning motion along the axis of the initial ice micro / nano fiber.

[0010] The initial ice micro-nano optical fiber was prepared by growing water vapor in the air within a temperature range of -50 ℃ to -30 ℃ using a high-voltage electric induction method, and its diameter was 1-10 μm.

[0011] The first and second fiber clamps are both quartz optical fibers with flattened end faces, and the first and second fiber clamps are kept on the same straight line axially.

[0012] The output wavelength of the infrared light source is >1 μm.

[0013] The quartz fiber taper has a tip diameter of 1-5 μm and is used to localize the infrared light energy emitted by the infrared light source on the processing area of ​​the initial ice micro-nano fiber.

[0014] III. A method for fabricating submicron diameter ice micro / nano optical fibers, the method comprising the following steps: S1: The initial ice micro-nano fiber is clamped and fixed by the first fiber clamp and the second fiber clamp, so that one end of it is suspended in the air. S2: Activate the infrared light source. The infrared light emitted by the infrared light source is conducted through the quartz fiber cone and output to illuminate the suspended end of the initial ice micro-nano fiber. S3: Control the quartz fiber taper to perform uniform or variable speed scanning motion along the axis of the initial ice micro / nano fiber. S4: By adjusting the output power of the infrared light source and using a precision displacement stage to control the scanning speed of the quartz fiber taper, the suspended end of the initial ice micro / nano fiber is locally heated, causing controllable vaporization and sublimation of the surface, thereby achieving controllable reduction in diameter, and finally obtaining the submicron diameter ice micro / nano fiber as described in claim 1.

[0015] In step S4, the output power of the infrared light source is in the range of 1-10 mW, and the scanning speed of the quartz fiber taper is in the range of 0.1-100 μm / s.

[0016] The method is performed in a low-temperature environment below -50 °C.

[0017] Based on the strong absorption characteristics of ice in the infrared band, this invention uses a quartz fiber taper to conduct infrared light energy and precisely controls the light intensity and scanning speed to achieve local heating of a specific area of ​​the initial ice micro / nano fiber, causing it to undergo a controllable vaporization and sublimation process, thereby reducing the diameter of the ice fiber to the submicron scale and producing ice micro / nano fibers with a diameter between 10 and 500 nm.

[0018] Compared with the prior art, the beneficial effects of the present invention are: (1) Breakthrough in size limitation: This invention abandons the traditional idea of ​​"direct growth" and innovatively proposes a secondary refinement strategy of "grow first, then process". It directly manufactures the initial ice micro-nano fiber by thermally induced sublimation, and successfully realizes the controllable preparation of submicron diameter ice micro-nano fiber, thus solving the technical bottleneck of traditional methods.

[0019] (2) High processing precision and strong controllability: By using a quartz fiber taper to localize light energy in a very small area, spatial selective heating at the nanoscale is achieved. By precisely controlling the two key parameters of infrared light power and scanning speed, the diameter, length and uniformity of the final submicron diameter ice micro-nano fiber can be controlled with high precision, and the repeatability is good.

[0020] (3) The prepared optical fiber has excellent quality: Since the diameter reduction is achieved by uniform sublimation of surface material, the prepared submicron diameter ice micro-nano optical fiber has a smooth surface, good diameter uniformity, and complete crystal structure. It has excellent mechanical properties and low-loss single-mode optical waveguide characteristics, providing an ideal material for the construction of high-performance ice-based photonic devices.

[0021] (4) The method and apparatus are simple and reliable: The apparatus has a simple structure and can be built with only a conventional fiber optic operating platform and optical components. The method has a clear process and is easy to operate, avoiding complex growth environment control and uncertain growth factors, thus improving the success rate and efficiency of preparation.

[0022] In summary, the method of this invention is simple in process and has high control precision, enabling stable fabrication of submicron diameter ice micro / nano optical fibers that were previously difficult to achieve. The fabricated submicron diameter ice micro / nano optical fibers have smooth surfaces, good diameter uniformity, and adjustable diameter and uniform region length. They possess excellent mechanical properties and low-loss single-mode waveguide capability, providing a key material foundation for the field of low-temperature photonics and micro / nano optical devices. Attached Figure Description

[0023] Figure 1 This is a schematic diagram of a submicron diameter ice micro / nano fiber structure and fabrication device according to the present invention; In the figure: 1-Initial ice micro / nano fiber, 2-First fiber holder, 3-Second fiber holder, 4-Infrared light source, 5-Quartz fiber taper, 6-Precision displacement stage, 7-Submicron diameter ice micro / nano fiber.

[0024] Figure 2 The experiment demonstrates the results of fabricating submicron-diameter ice micro / nano fibers with a diameter of approximately 500 nm by photothermal induction treatment from initial ice micro / nano fibers with a diameter of 1.6 μm and a length of 34 μm. The left side of the figure shows the initial ice micro / nano fiber, and the right side shows the fabricated submicron-diameter ice micro / nano fiber. Detailed Implementation

[0025] The technical solution of the present invention will be described in detail below with reference to the accompanying drawings and specific embodiments, but the scope of protection of the present invention is not limited thereto.

[0026] like Figure 1 As shown, the device includes an initial ice micro / nano fiber 1, a first fiber clamp 2, a second fiber clamp 3, an infrared light source 4, and a quartz fiber taper 5. The initial ice micro / nano fiber 1 can be arranged horizontally, clamped and fixed by the first fiber clamp 2 and the second fiber clamp 3, with one end suspended. One end of the quartz fiber taper 5 is connected to the infrared light source 4, and one end of the infrared light source 4 is used to provide the light energy required for processing. The other end of the quartz fiber taper 5 is fixed on a precision displacement stage 6, arranged in a direction perpendicular to the axis of the initial ice micro / nano fiber 1 and facing the suspended end of the initial ice micro / nano fiber 1. The quartz fiber taper 5 can perform scanning motion along the axis of the initial ice micro / nano fiber 1.

[0027] The quartz fiber taper 5 can be arranged in a scanning motion along the axis of the initial ice micro / nano fiber 1. The tip diameter of the quartz fiber taper 5 is 1-5 μm, which is used to localize the infrared light energy emitted by the infrared light source 4 on the small processing area of ​​the initial ice micro / nano fiber 1.

[0028] In practice, the initial ice micro / nano fiber 1 is prepared by growing water vapor in the air within a temperature range of -50 ℃ to -30 ℃ using a high-voltage electro-induced method, and its diameter is 1-10 μm. The output wavelength of the infrared light source 4 is >1 μm.

[0029] The first fiber clamp 2 and the second fiber clamp 3 are standard quartz optical fibers with flattened end faces, and the first fiber clamp 2 and the second fiber clamp 3 are kept on the same straight line axially.

[0030] The preparation process using the apparatus of this invention includes the following steps: S1: The initial ice micro-nano fiber 1 is clamped and fixed by the first fiber clamp 2 and the second fiber clamp 3, so that one end of it is suspended in the air; S2: Start the infrared light source 4. The infrared light emitted by the infrared light source 4 is conducted through the quartz fiber cone 5 and output to illuminate the suspended end of the initial ice micro-nano fiber 1. S3: Control the quartz fiber taper 5 to perform uniform or variable speed scanning motion along the axis of the initial ice micro-nano fiber 1. S4: By adjusting the output power of the infrared light source 4 and using the precision displacement stage 6 to control the scanning speed of the quartz fiber taper 5, the output power can be adjusted by an adjustable attenuator or knob. This allows for local heating of the suspended end of the initial ice micro-nano fiber 1, causing its surface to undergo controllable vaporization and sublimation, thereby achieving controllable reduction in diameter and finally obtaining the submicron diameter ice micro-nano fiber 7 of claim 1.

[0031] In step S4, the output power of the infrared light source 4 is in the range of 1-10 mW, and the scanning speed of the quartz fiber taper 5 is in the range of 0.1-100 μm / s.

[0032] The above process is carried out in a low-temperature environment below -50 °C to prevent the submicron diameter ice micro-nano fiber 7 from unexpected melting or structural damage during processing.

[0033] Example: Fabrication of a submicron diameter ice micro / nano optical fiber 1. Setup of the apparatus and preparation of initial materials First, set it up as shown in the attached diagram. Figure 1 The preparation apparatus shown is mainly composed of: Initial ice micro / nano fiber 1: A single-crystal ice micro / nano fiber with a diameter of about 1.6 μm and a length of about 50 μm was prepared as a processing raw material by high voltage electro-induced growth method in an environment of -40°C and supersaturated humidity.

[0034] First and second fiber clamps 2 and 3: Two standard quartz optical fibers with flattened end faces are used as clamps to clamp the end of the initial ice micro-nano fiber 1, making it suspended in the air.

[0035] Infrared source 4: A continuous semiconductor laser with an output wavelength of 1550 nm is selected. This wavelength is near the intrinsic absorption peak of ice material. The output power of the laser is adjustable from 1 to 10 mW.

[0036] Quartz fiber taper 5: A quartz fiber taper with a tip diameter of approximately 2 μm was prepared using the flame stretching method.

[0037] The output pigtail of the infrared light source 4 is connected to the thicker end of the quartz fiber taper 5 via a fiber optic connector. The other end of the quartz fiber taper 5 is fixed to the precision displacement stage 6.

[0038] The entire device is placed in a temperature-controlled cryogenic chamber, and the ambient temperature is kept stable at -80 °C to prevent the ice fiber from melting during processing.

[0039] 2. Photothermal-induced fine processing S1: Turn on the infrared light source 4 and adjust its output power to 5 mW. After being transmitted through the quartz fiber taper 5, the infrared laser is output from the tip of the quartz fiber taper 5 and illuminates the initial ice micro-nano fiber 1 in front; S2: Control the quartz fiber taper 5 through the precision displacement stage 6, so that its taper tip approaches the fiber surface in a direction perpendicular to the axis of the initial ice micro-nano fiber 1, until it enters the optical field action area.

[0040] S3: Drive the precision displacement stage 6 to make the quartz fiber cone 5 perform uniform or variable speed scanning motion along the axis of the initial ice micro-nano fiber, with a scanning speed of 10 μm / s.

[0041] S4: During the scanning process, infrared light is strongly absorbed by the initial ice micro / nano fiber 1 and converted into heat energy, generating local high temperatures in the interaction area, causing the ice material to undergo controllable vaporization and sublimation. This process results in a uniform and precise reduction in the fiber diameter, ultimately producing a submicron diameter ice micro / nano fiber 7.

[0042] 3. Results and Characterization After the above processing steps, the initial ice micro / nano fiber was transformed into a uniform submicron diameter ice micro / nano fiber. (See attached image.) Figure 2 As shown, the initial ice micro-nano fiber region (left side) before processing has a diameter of about 1.6 μm, while the region after photothermal induction treatment (right side) has a diameter that is uniformly reduced to about 500 nm, with a smooth surface and a gentle transition region.

[0043] As demonstrated in this embodiment, this invention utilizes the strong absorption characteristics of ice micro / nano fibers in the infrared band and innovatively employs a photothermal-induced local sublimation method to successfully achieve nanoscale precision processing of initial ice micro / nano fibers, fabricating submicron diameter ice micro / nano fibers with diameters as low as 500 nm or even finer. This method is simple, precisely controlled, and highly repeatable, effectively overcoming the technical bottleneck of traditional growth methods in the controllable fabrication of submicron diameter ice fibers.

[0044] The specific embodiments described above are intended to explain and illustrate the technical solutions of the present invention and do not constitute any limitation on the scope of protection of the present invention. Within the core principles disclosed in the present invention and the scope of protection defined by the claims, any equivalent substitutions, obvious modifications, and further optimizations based on the present invention are included within the scope of the present invention patent application.

Claims

1. A submicron diameter ice micro / nano optical fiber, characterized in that, The submicron diameter ice micro-nano fiber (7) has a diameter of 10-500 nm and is obtained by thermally induced sublimation of the initial ice micro-nano fiber (1).

2. An apparatus for fabricating the submicron diameter ice micro / nano optical fiber of claim 1, characterized in that: The device includes an initial ice micro-nano fiber (1), a first fiber holder (2), a second fiber holder (3), an infrared light source (4), and a quartz fiber taper (5). The initial ice micro-nano fiber (1) is clamped and fixed by the first fiber holder (2) and the second fiber holder (3) and one end is suspended. One end of the quartz fiber taper (5) is connected to the infrared light source (4), and one end of the infrared light source (4) is used to provide the light energy required for processing. The other end of the quartz fiber taper (5) is fixed on a precision displacement stage (6) and arranged in a direction perpendicular to the axis of the initial ice micro-nano fiber (1) and facing the end of the initial ice micro-nano fiber (1) that is suspended.

3. The apparatus for fabricating submicron diameter ice micro / nano optical fibers according to claim 2, characterized in that: The quartz fiber taper (5) can be arranged in a scanning motion along the axis of the initial ice micro-nano fiber (1).

4. The apparatus for fabricating submicron diameter ice micro / nano optical fibers according to claim 2, characterized in that: The initial ice micro-nano fiber (1) is prepared by growing water vapor in the air as raw material in the temperature range of -50 ℃ to -30 ℃ using a high voltage electric induction method, and its diameter is 1-10 μm.

5. The apparatus for fabricating submicron diameter ice micro / nano optical fibers according to claim 2, characterized in that: The first optical fiber holder (2) and the second optical fiber holder (3) are respectively quartz optical fibers with flattened end faces, and the first optical fiber holder (2) and the second optical fiber holder (3) are kept on the same straight line axially.

6. The apparatus for fabricating submicron diameter ice micro / nano optical fibers according to claim 2, characterized in that: The output wavelength of the infrared light source (4) is >1 μm.

7. The apparatus for fabricating submicron diameter ice micro / nano optical fibers according to claim 2, characterized in that: The quartz fiber taper (5) has a taper diameter of 1-5 μm and is used to localize the infrared light energy emitted by the infrared light source (4) on the processing area of ​​the initial ice micro-nano fiber (1).

8. A method for fabricating submicron diameter ice micro / nano optical fibers using the device described in any one of claims 2 to 7, characterized in that, The method includes the following steps: S1: The initial ice micro-nano fiber (1) is clamped and fixed by the first fiber clamp (2) and the second fiber clamp (3), so that one end of it is suspended in the air; S2: Start the infrared light source (4). The infrared light emitted by the infrared light source (4) is conducted through the quartz fiber cone (5) and output to irradiate the suspended end of the initial ice micro-nano fiber (1). S3: Control the quartz fiber taper (5) to perform uniform or variable speed scanning motion along the axis of the initial ice micro-nano fiber (1). S4: By adjusting the output power of the infrared light source (4) and using the precision displacement stage (6) to control the scanning speed of the quartz fiber taper (5), the suspended end of the initial ice micro-nano fiber (1) is locally heated, so that the surface undergoes controllable vaporization and sublimation, thereby achieving controllable reduction in diameter, and finally obtaining the submicron diameter ice micro-nano fiber (7) as described in claim 1.

9. The method for preparing submicron diameter ice micro / nano optical fibers according to claim 8, characterized in that: In step S4, the output power of the infrared light source (4) is in the range of 1-10 mW, and the scanning speed of the quartz fiber taper (5) is in the range of 0.1-100 μm / s.

10. The method for preparing submicron diameter ice micro / nano optical fibers according to claim 8, characterized in that: The method is performed in a low-temperature environment below -50 °C.