Low-loss organic ice micro-nano optical fiber and preparation method thereof
By adding organic liquid between standard quartz single-mode optical fibers and stretching them to form organic ice micro-nano optical fibers, the difficulty in preparing high-quality, low-loss optical fibers was solved, and optical fibers with low loss and high mechanical properties were achieved, which are suitable for the research of organic ice and measurements in extreme environments.
Patent Information
- Application Number
- CN202411694567.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-25
- Publication Date
- 2025-10-10
- Estimated Expiration
- 2044-11-25
AI Technical Summary
It is difficult to prepare high-quality, low-loss organic ice micro-nano optical fibers with existing technologies, especially crystalline optical fibers, which have problems of high light scattering loss and propagation loss over longer lengths.
Two standard quartz single-mode optical fibers are placed at intervals, an organic liquid is added, and the temperature is lowered to near the glass transition temperature. Low-loss organic ice micro-nano optical fibers are formed by stretching. The temperature and stretching speed are controlled to ensure a smooth surface and uniform diameter.
High-quality organic ice micro-nano optical fibers with low loss, smooth surface and uniform diameter are achieved. They are suitable for a variety of organic liquids and mixed solutions, have low transmission loss and good mechanical properties, are suitable for extreme environments, and are suitable for waveguide and extreme mechanical property measurements.
Smart Images
Figure CN119575539B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of waveguide preparation, and in particular to a low-loss organic ice micro-nano optical fiber and a preparation method thereof. Background Art
[0002] Small organic molecules such as alkanes, alcohols, and benzenes are widely present in the universe. Unlike the common liquid and gaseous forms on Earth, in regions of the universe with more extreme conditions, many small organic molecules exist in solid form, which is called organic ice. For example, in the solar system, the average surface temperature of Mars is about -65°C, and as the distance from the sun increases, the average surface temperature of the planet will drop further. Since the optical properties of organic ice, such as infrared and ultraviolet spectra and polarization spectra, are extremely important for understanding the material environment of interstellar space and the evolution of celestial bodies, exploring its basic optical properties such as refractive index and absorption is of great significance.
[0003] Micro-nano optical fibers are one-dimensional optical waveguides with diameters close to or smaller than the wavelength of the light they transmit. They offer advantages such as low transmission loss, strong optical field confinement, strong evanescent fields, and surface field enhancement, making them suitable for exploring the extreme physical and chemical properties of materials. Leveraging this highly flexible and versatile research platform, the development of organic ices as micro-nanoscale one-dimensional waveguides can advance organic ice research, deepen understanding of their mechanical and optical properties, and open up new possibilities for organic ice-based technologies.
[0004] Micro-nano optical fibers can be categorized as amorphous and crystalline, respectively, with disordered and ordered structures, exhibiting distinct optical and mechanical properties, suitable for diverse research and applications. Crystalline optical fibers, due to the inevitable introduction of defects during their growth process, exhibit higher light scattering and propagation losses. The growth rate of crystalline fibers is generally lower than the stretching rate of amorphous fibers. At longer lengths (e.g., >1 cm), achieving high quality with crystalline fibers is more challenging. Summary of the Invention
[0005] In order to solve the problems existing in the background technology, the present invention provides a low-loss organic ice micro-nano optical fiber and a preparation method thereof, which can better prepare high-quality one-dimensional organic ice micro-nano optical fiber with smooth surface, uniform diameter and low loss.
[0006] The organic ice micro-nano optical fiber prepared by the present invention provides a new platform for studying the physical and chemical properties of organic small molecules and expanding their applications as functional materials. It has great research and practical value in the fields of physical chemistry, materials science, life science and space exploration.
[0007] To achieve the above object, the technical solution adopted by the present invention is as follows:
[0008] 1. A method for preparing low-loss organic ice micro-nano optical fiber, the method comprising the following steps:
[0009] S1: Two standard single-mode quartz optical fibers are placed along a straight line with a gap between their adjacent ends serving as a sample preparation area. An organic liquid is dripped into the gap between the two quartz single-mode optical fibers to smoothly fill the gap. Ultimately, the adjacent ends of the two quartz optical fibers are connected by the organic liquid, i.e., the dripped organic liquid is connected to the adjacent end faces of the two quartz optical fibers.
[0010] S2: using a cooling material to lower the temperature of the sample preparation area to near the glass transition temperature of the added organic liquid, and slightly adjusting the temperature of the sample preparation area to be slightly higher than the glass transition temperature, so that the added organic liquid is in a highly viscous supercooled state;
[0011] S3: Pull the two standard quartz single-mode optical fibers in opposite directions at a uniform speed, thereby stretching the viscous organic liquid added until a uniform area of organic ice micro-nano optical fibers that meets the use length requirements is clearly seen, thereby obtaining high-quality one-dimensional organic ice micro-nano optical fibers, which still need to be kept at low temperatures during storage and use.
[0012] In step S1, the size of the sample preparation area is several tens of micrometers to 100 micrometers.
[0013] In step S2, liquid nitrogen is used as the cooling material, and the sample preparation area is placed in a clean cold nitrogen atmosphere with adjustable temperature. The speed of lowering the temperature of the sample preparation area is greater than 50°C / s, and the temperature of the sample preparation area is slightly higher than the glass transition temperature of the organic liquid, about 0-15°C.
[0014] In step S3, the standard quartz single-mode optical fiber is uniformly pulled at a speed of 0.05-1 mm / s.
[0015] Preferably, the proportion of the uniform area of the organic ice micro-nano optical fiber can be adjusted by adjusting the temperature of the sample preparation area and the speed of stretching the organic liquid.
[0016] In the step S1, the organic liquid is a glassy organic liquid or a binary mixed solution that can achieve glass transition.
[0017] The preparation method described in the present invention has been shown to be applicable to organic compound liquids such as methanol, ethanol, ethylene glycol, glycerol, glycerol, toluene, ethylbenzene, benzyl acetate, etc.; it is also applicable to organic binary mixed solutions, more specifically, organic binary mixed solutions such as chloroform-ethylbenzene (60:40), tetrachloromethane-ethylbenzene (50:50) and carbon disulfide-toluene (80:20), which are mixed in a specified molar ratio.
[0018] In step S3, the organic ice micro-nano optical fiber uniform region is a cylindrical region with uniform diameter between the two end cone regions formed after the organic liquid is stretched.
[0019] 2. Low-loss organic ice micro-nano optical fiber: The organic ice micro-nano optical fiber prepared by the preparation method has a uniform diameter and a smooth surface. The diameter can be from sub-wavelength to 10 μm, the length can reach several centimeters, and the root mean square roughness of the surface is less than 0.5 nm.
[0020] 3. An application of the organic ice micro-nano optical fiber in wave guiding, optical property measurement of organic small molecule substances and extreme mechanical property measurement.
[0021] 4. A detection method for organic ice micro-nano optical fiber:
[0022] The method is:
[0023] Before or after the preparation of the organic ice micro-nano optical fiber is completed, the ends of two standard quartz single-mode optical fibers that are separated from each other are connected to the light source and the spectrometer respectively. The temperature of the sample preparation area is maintained below the glass transition temperature of the added organic liquid and above the liquid nitrogen temperature for waveguide measurement.
[0024] Preferably, the specific requirements for the temperature of the sample preparation area are determined by the test requirements. When performing single-wavelength waveguide measurement, the end of the quartz fiber on one side is connected to a supercontinuum light source, combined with a wavelength bandwidth tunable filter (wavelength of about 400-800nm, single wavelength output, bandwidth of about 5-50nm adjustable), and the other side is connected to a spectrometer (wavelength 600-1700nm, resolution 0.05nm, maximum power +20dBm (100mW)). When performing broadband waveguide measurement, the end of the quartz fiber on one side is connected to a high-brightness broadband light source (wavelength 190-2100nm, NA = 0.22, 150mW), and the other side is connected to the same spectrometer as above. By analyzing the image of the microscope system and the data collected by the spectrometer, the detection results of the low-loss characteristics of the organic ice fiber are obtained.
[0025] The present invention has the following beneficial effects:
[0026] (1) The method of the present invention is the first to achieve the preparation of a variety of new small molecule organic micro-nano optical fibers with smooth surfaces and uniform diameters, with the surface root mean square roughness less than 0.5 nm;
[0027] (2) The present invention can achieve precise control over the diameter and length of the uniform zone over a wide range, wherein the diameter can be controlled from the sub-wavelength level to 10 μm and the length can reach several centimeters;
[0028] (3) The preparation method of the organic ice micro-nano optical fiber of the present invention is applicable to a wide range of raw materials, and is applicable to a variety of organic liquids in a glassy state, and is also applicable to a variety of binary mixed solutions that can achieve glass transition;
[0029] (4) The two ends of the organic ice micro-nano optical fiber in the present invention are naturally connected to the quartz optical fiber, and the light field can be efficiently coupled into and out of the organic ice micro-nano optical fiber through the standard quartz optical fiber, realizing optical measurement and application;
[0030] (5) The organic ice micro-nano optical fiber prepared by the present invention can achieve low transmission loss in a wide band, with the minimum loss being less than 0.03 dB / cm;
[0031] (6) The organic ice micro-nano optical fiber prepared by the method of the present invention has good mechanical properties, low defect density and high structural uniformity, and thus has high toughness;
[0032] (7) Organic small molecules are ubiquitous in extraterrestrial planets or the universe and have been shown to have good stability in these extreme environments (extremely low temperatures, cosmic ray radiation, etc.). Therefore, the optical fiber prepared directly using organic small molecules in the present invention has universal adaptability to the environment and can still maintain its ability to bend and stretch freely at temperatures below 100K.
[0033] (8) The organic ice micro-nano optical fiber prepared by the method of the present invention has a fast preparation speed and is easy to obtain a long and uniform structure. The stretching preparation speed is 0.05-1 mm / s.
[0034] (9) The organic ice micro-nano optical fiber prepared by the present invention can realize active doping and low-threshold supercontinuum generation based on the advantages of organic materials such as dopability and high nonlinear coefficient. BRIEF DESCRIPTION OF THE DRAWINGS
[0035] Figure 1 It is a schematic diagram of the structure of a device suitable for the method for preparing organic ice micro-nano optical fibers of the present invention.
[0036] Figure 2 This is an optical microscope photo of the ethanol ice optical fiber stretching process.
[0037] Figure 3 This is a schematic diagram of the device for waveguide measurement of organic ice micro-nano optical fibers.
[0038] Figure 4 This is a dark-field micrograph of laser light transmitted through an ethanol ice fiber.
[0039] Figure 5 This is a diagram of the broadband transmission characteristics of ethanol ice optical fibers with different diameters.
[0040] In the figure: 1. Microscope system, 2. Standard quartz single-mode optical fiber, 3. Motorized translation stage, 4. Cold chamber, 5. Transparent viewing window, 6. Liquid nitrogen, 7. Lifting platform, 8. Temperature measuring line, 9. Pipette, 10. Organic liquid, 11. Fiber optic clamp, 12. Light source, 13. Spectrometer. DETAILED DESCRIPTION
[0041] The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments, but the present invention is not limited to the following embodiments.
[0042] The embodiments of the present invention are as follows:
[0043] Example 1
[0044] This embodiment assembles a preparation device suitable for the preparation method of the present invention. The structural diagram of this preparation device is shown in FIG. Figure 1 As shown, the preparation device includes a microscope system 1, a standard quartz single-mode optical fiber 2, a motorized translation stage 3, a cold chamber 4, a transparent viewing window 5, a lifting platform 7, a thermocouple temperature measuring line 8 and an optical fiber clamp 11;
[0045] A transparent viewing window 5 with two symmetrical through-holes is mounted on the top surface of the cold chamber 4. A microscope system 1 is mounted directly above the transparent viewing window 5 via an external support arm, with its lens facing the window 5. A motorized translation stage 3 is symmetrically positioned on either side of the cold chamber 4, each with a fiber clamp 11 affixed to it. Two standard single-mode quartz optical fibers 2 are secured to the two fiber clamps 11 using UV-curable adhesive. Together with the fiber clamps 11, the standard single-mode quartz optical fibers 2 pass through the through-holes in the transparent viewing window 5 and are freely inserted into the cold chamber 4. Within the cold chamber 4, the two standard single-mode quartz optical fibers 2 are placed parallel to each other and face each other end-to-end.
[0046] A cold chamber 4 is placed on a lifting platform 7 and contains a cooling material, liquid nitrogen 6. In the initial state of the preparation device, an adjustable gap, ranging from tens to 100 microns, is provided between the ends of two standard single-mode quartz optical fibers 2 within the cold chamber 4, serving as a sample preparation area. The sample preparation area is placed within the field of view of a microscope system 1, which can observe and record the preparation process in the sample preparation area in real time through a transparent viewing window 5. The probe of a thermocouple temperature measuring line 8 is suspended in the air and close to the end face of the standard single-mode quartz optical fiber 2, monitoring the temperature near the sample preparation area in real time. By adjusting the height of the lifting platform 7, that is, adjusting the vertical distance between the liquid nitrogen 6 level and the standard single-mode quartz optical fiber 2, the temperature of the sample preparation area can be changed or maintained for a long period of time.
[0047] The preparation device further includes a pipette 9 for extending into the cold chamber 4 to drip an organic liquid 10 .
[0048] The method for preparing organic ice micro-nano optical fiber using the preparation device includes the following steps:
[0049] (1) First, adjust the height of the lifting platform 7 to the lowest, remove the cold chamber 4, glue a standard quartz single-mode optical fiber 2 on each optical fiber clamp 11, and place the proximal end areas of the two standard quartz single-mode optical fibers 2 along the same straight line. There is a gap between the adjacent ends of the two standard quartz single-mode optical fibers 2 as a sample preparation area. Add liquid nitrogen 6 with a liquid level lower than that of the standard quartz single-mode optical fibers 2 into the cold chamber 4, and then put the cold chamber 4 back on the lifting platform 7. At this time, the environment near the standard quartz single-mode optical fibers 2 is at room temperature, and the part inside the cold chamber 4 is in a clean cold nitrogen atmosphere with adjustable temperature;
[0050] (2) A small amount of organic liquid is sucked through the pipette 9, and then the pipette 9 is extended into the cold chamber 4, and a drop of organic liquid 10 is dripped into the sample preparation area, and the sample preparation area is smoothly filled by the surface tension of the organic liquid 10;
[0051] (3) By raising the height of the lifting platform 7 to drive the cold chamber 4, the vertical distance between the liquid nitrogen 6 and the standard quartz single-mode optical fiber 2 is adjusted, thereby lowering the temperature of the sample preparation area to near the glass transition temperature of the added organic liquid, and fine-tuning the temperature of the sample area to be slightly higher than the glass transition temperature, so that the added organic liquid is in a highly viscous supercooled state;
[0052] (4) The standard quartz single-mode optical fiber 2 is moved in the opposite direction at a uniform speed by the electric translation stage 3, thereby stretching the added organic liquid 10 until a uniform region of organic ice micro-nano optical fiber that meets the use length requirement is clearly present, thereby obtaining the organic ice micro-nano optical fiber.
[0053] Example 2
[0054] This embodiment provides a specific implementation process of preparing ethanol ice optical fiber using the preparation method of the present invention. The stretching process of ethanol ice optical fiber near -175℃ is as follows: Figure 2 As shown in the figure, during the stretching process, as the stretching length increases, the diameter of the ethanol ice fiber gradually decreases. The connection between the ethanol ice fiber and the quartz fiber is a conical area with a drastic change in diameter, and the middle is a uniform diameter area. The stretching speed of ethanol shown in the figure is 0.3 mm / s.
[0055] Example 3
[0056] This embodiment provides a specific implementation process for quality inspection of the organic ice micro-nano optical fiber obtained by the preparation method of the present invention. In order to characterize its light field transmission characteristics such as loss, before or after the preparation of the organic ice micro-nano optical fiber, a light source 12 and a spectrometer 13 can be connected to the outer ends of two standard quartz single-mode optical fibers to perform waveguide measurement. The schematic diagram of the device for waveguide measurement is shown in FIG. Figure 3As shown, the light field is efficiently coupled into the organic ice fiber through the left quartz fiber, and then collected by the right quartz fiber into the spectrometer 13. By analyzing the image of the microscope system 1 and the data collected by the spectrometer 13, the low-loss characteristics of the organic ice fiber can be detected.
[0057] The microscope system test results are as follows Figure 4 As shown, Figure 4 These dark-field micrographs show the organic ice fiber transmitting laser beams at 475nm, 500nm, 525nm, 550nm, 575nm, and 600nm wavelengths. The dark-field micrographs show no apparent surface scattering of the organic ice fiber. Strong scattering occurs only at the output end, where light enters the coupling region from the organic ice fiber to the quartz fiber. At the input end, where light enters the coupling region from the quartz fiber to the organic ice fiber, light scattering is weak, indicating that light efficiently enters the organic ice fiber.
[0058] The spectrometer test results are as follows Figure 5 As shown, Figure 5 The broadband transmission characteristics of organic ice fibers with different diameters are shown. The wavelength range of the broadband light is 400-1550 nm. Due to the cutoff of higher-order modes, the transmission power decreases as the diameter of the organic ice fiber decreases.
[0059] The above specific embodiments are used to illustrate the present invention rather than to limit the present invention. Any modifications and changes made to the present invention within the spirit of the present invention and the protection scope of the claims shall fall within the protection scope of the present invention.
[0060] The above description is only a preferred embodiment of the present invention. Therefore, any equivalent changes or modifications made according to the structure, characteristics and principles described in the scope of the patent application of the present invention are included in the scope of the patent application of the present invention.
Claims
1. A method for preparing low-loss organic ice micro-nano optical fiber, characterized by: The method comprises the following steps: S1: Place two quartz single-mode optical fibers along the same straight line with a gap between their adjacent ends as a sample preparation area. Drop an organic liquid into the gap between the quartz single-mode optical fibers to smoothly fill the gap. S2: using a cooling material to lower the temperature of the sample preparation area to near the glass transition temperature of the added organic liquid, and adjusting the temperature of the sample preparation area to be higher than the glass transition temperature; S3: The two quartz single-mode optical fibers are pulled at a constant speed in opposite directions, thereby stretching the added organic liquid until a uniform region of organic ice micro-nano optical fibers that meets the use length requirements appears, thereby obtaining an organic ice micro-nano optical fiber.
2. The method for preparing a low-loss organic ice micro-nano optical fiber according to claim 1, characterized in that: In step S1, the size of the sample preparation area is several tens of micrometers to 100 micrometers.
3. The method for preparing a low-loss organic ice micro-nano optical fiber according to claim 1, characterized in that: In step S2, liquid nitrogen is used as the cooling material, the speed of reducing the temperature of the sample preparation area is greater than 50°C / s, and the temperature of the sample preparation area is 0-15°C higher than the glass transition temperature of the organic liquid.
4. The method for preparing a low-loss organic ice micro-nano optical fiber according to claim 1, characterized in that: In step S3, the quartz single-mode optical fiber is uniformly pulled at a speed of 0.05-1 mm / s.
5. The method for preparing a low-loss organic ice micro-nano optical fiber according to claim 1, characterized in that: In the step S1, the organic liquid is a glassy organic liquid or a binary mixed solution that can achieve glass transition.
6. The method for preparing a low-loss organic ice micro-nano optical fiber according to claim 1, characterized in that: In step S3, the organic ice micro-nano optical fiber uniform region is a cylindrical region with uniform diameter between the two end cone regions formed after the organic liquid is stretched.
7. A low-loss organic ice micro-nano optical fiber, characterized by: The invention is prepared by the preparation method according to any one of claims 1 to 6.
8. Application of the organic ice micro-nano optical fiber prepared by the preparation method according to any one of claims 1 to 6 in wave guiding, measurement of optical properties of organic small molecules, and measurement of ultimate mechanical properties.
9. A method for detecting an organic ice micro-nano optical fiber produced by the preparation method according to any one of claims 1 to 6.
10. The detection method according to claim 9, characterized in that: The method is as follows: before or after the preparation of the organic ice micro-nano optical fiber is completed, the ends of two quartz single-mode optical fibers that are far away from each other are connected to a light source and a spectrometer respectively, the temperature of the sample preparation area is maintained below the glass transition temperature of the added organic liquid and above the liquid nitrogen temperature, and waveguide measurement is performed.