A preparation method for a quartz fiber sample used in electron probe testing

Abstract

The present invention discloses a method for preparing a quartz optical fiber sample for electronic probe testing, which includes an optical fiber carrier provided with an optical fiber groove matching the optical fiber to be tested. The preparation method includes the following steps: firstly, judging the diameter of the optical fiber to be tested, selecting an appropriate cutter for cutting, and during cutting, the optical fiber cutting angle is not greater than 1.5°; selecting an optical fiber carrier adapted to the diameter of the optical fiber to be tested, and transferring the cut optical fiber to be tested to the optical fiber groove of the optical fiber carrier adapted to the optical fiber carrier; pushing the optical fiber to be tested from the cut end face of the optical fiber to be tested so that the cut end face of the optical fiber to be tested is flush with the upper end face of the optical fiber carrier; using a conductive tape to stick across the entire end face of the optical fiber carrier provided with the optical fiber to be tested, and the sticking position of the conductive tape is set lower than the end face of the optical fiber carrier; placing the optical fiber carrier with the optical fiber stuck thereon into a vacuum carbon coating instrument for carbon coating.

Description

Technical Field

[0001] The invention relates to the technical field of optical fiber testing, in particular to a method for preparing a quartz optical fiber sample for electronic probe testing. Background Art

[0002] Electron probe microanalyzers can be used to measure and analyze the content of doping elements in solid materials and are widely used in material content testing. Standards such as "GB / T15074-2008 General Rules for Electron Probe Quantitative Analysis Methods" and "GB / T15617-2002 Electron Probe Quantitative Analysis Methods for Silicate Minerals" describe methods for electron probe analysis of materials. The core of a quartz optical fiber is typically located at the geometric center of the fiber. Doping elements increase the core's refractive index, forming a waveguide structure. Common communication optical fibers typically have a diameter of 125 μm and a core diameter of 9 μm. Common specialty optical fibers typically have diameters of 250 μm, 400 μm, and so on.

[0003] To achieve optimal testing results, the quartz fiber's analytical surface must be level and have good electrical conductivity. Compared to common solid materials like silicate minerals, quartz fiber has a very small diameter. Therefore, securing the quartz fiber and ensuring a level analytical surface is crucial for optimal testing results.

[0004] Currently, there are no specific electronic probe testing methods for optical fibers. Traditional methods, particularly for very small test samples, typically employ methods such as sample embedding. Several optical fiber samples are placed in a plastic tube, filled with curing glue and a curing agent (such as epoxy resin or a curing agent), and then embedded within. The embedded fibers, along with the curing agent, are then ground on a grinder until the surface is smooth and scratch-free. The samples are then carbon-plated.

[0005] However, this method involves a long sample preparation cycle, involving steps such as mounting, curing, grinding, and polishing. Typically, this can take more than a day. Furthermore, due to issues with fiber placement and the flow of curing adhesive, it's difficult to ensure the fiber is vertically aligned during mounting. Consequently, the electron probe microanalyzer displays the fiber as an oblique cross-section, making it impossible to accurately measure parameters such as fiber diameter and ellipticity, and thus unable to accurately reflect the cross-sectional composition distribution of the fiber. Summary of the Invention

[0006] The purpose of the present invention is to provide a method for preparing quartz optical fiber samples for electronic probe testing in response to the above problems, which solves the problems in the prior art of long sample preparation time, inability to accurately test parameters such as the diameter and ellipticity of the optical fiber after sample preparation, and inability to accurately reflect the cross-sectional component distribution of the optical fiber.

[0007] The present invention is achieved through the following solutions:

[0008] A method for preparing a quartz optical fiber sample for electronic probe testing includes a fiber carrier provided with an optical fiber groove matching the size of the optical fiber to be tested; the preparation method includes the following steps:

[0009] Step 1: Select an appropriate cleaver according to the diameter of the optical fiber to be tested and cut the optical fiber to be tested. The cutting angle should not exceed 1.5°.

[0010] Step 2: Transfer the cut fiber to be tested to the fiber groove of the fiber carrier that matches it. When placing the fiber to be tested, the cut end face of the fiber to be tested protrudes from the end face of the fiber carrier.

[0011] Step 3: Push the optical fiber to be tested from its cleaved end face so that the cleaved end face of the optical fiber to be tested is flush with the upper end face of the optical fiber carrier;

[0012] Step 4: Use conductive tape to stick across the entire end face of the optical fiber carrier where the optical fiber to be tested is set, and tighten all the optical fibers to be tested. The sticking position of the conductive tape is lower than the end face of the optical fiber carrier;

[0013] Step 5: Place the optical fiber carrier with the optical fiber attached into a vacuum carbon coating apparatus for carbon coating. During the carbon coating process, the upper end surface of the optical fiber carrier faces the carbon end.

[0014] In step 1, when judging the diameter of the optical fiber to be tested, if the diameter of the optical fiber is not greater than 130 μm, a communication optical fiber cutter is used for cutting; if the diameter of the optical fiber is greater than 130 μm, a large-diameter optical fiber cutter is used for cutting. The optical fiber to be tested is cut using a cutting tool.

[0015] In step three, while pushing the optical fiber to be tested, the optical fiber to be tested is contacted along the cut surface or circumferential position of the optical fiber to be tested, and a force is applied along the length direction of the optical fiber groove to make the cut end surface of the optical fiber to be tested flush with the upper end surface of the optical fiber carrier.

[0016] In step 4, the conductive tape is 0 mm to 2 mm lower than the end surface of the optical fiber carrier.

[0017] The bottom of the optical fiber groove is a semicircle that matches the curvature of the optical fiber to be tested. When the optical fiber to be tested is placed in the optical fiber groove, the optical fiber to be tested fits the bottom of the optical fiber groove. The depth of the optical fiber groove should be at least 50% to 80% of the optical fiber diameter.

[0018] The optical fiber carrier is made of a non-magnetic metal material with good electrical conductivity.

[0019] The upper and lower surfaces of the optical fiber carrier are parallel, and the cross-section of the optical fiber carrier is square or rectangular.

[0020] The length of the optical fiber carrier is no more than 30 mm, and the height is no more than 30 mm.

[0021] A plurality of optical fiber grooves are evenly arranged on the optical fiber carrier, and each optical fiber groove is arranged perpendicular to the upper and lower surfaces of the optical fiber carrier.

[0022] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are:

[0023] 1. This method can significantly shorten the time required to prepare one or more samples. This method allows for the preparation of optical fiber samples, including cutting, mounting on a fiber carrier, and carbon coating, in under two hours. Unlike traditional sample preparation methods, the cutting and mounting processes take less than 10 minutes.

[0024] 2. The fiber cross-sectional information obtained through this solution is accurate. Because the fiber cleavage angle is no greater than 1.5 degrees, the cut end face represents the fiber cross-section, not the oblique cut surface. Therefore, the cross-sectional information (e.g., fiber core diameter, core circularity, etc.) of the fiber samples prepared by this technical solution is accurate.

[0025] 3. In this solution, since the optical fiber is installed in a fiber groove perpendicular to the optical fiber carrier, the optical fiber analysis surface is horizontal and the test effect is good.

[0026] 4. At the same time, since the optical fiber analysis surface is flush with the upper surface of the optical fiber carrier and is coated with conductive tape, the optical fiber carrier has good conductivity. Therefore, the optical fiber sample after carbon spraying has good conductivity. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 Schematic diagram of the three-dimensional structure of the optical fiber carrier of the present invention equipped with the optical fiber to be tested;

[0028] Figure 2 Schematic diagram of the cross-sectional structure of the optical fiber carrier of the present invention equipped with the optical fiber to be tested;

[0029] Figure 3 This is the core composition morphology diagram obtained by electron probe analysis after sample preparation using this method;

[0030] Figure 4 This is an optical microscope focus image of an electron probe after sample preparation using existing technology;

[0031] Figure 5 This is the focus image of the electron probe using an optical microscope after the sample is prepared using this method;

[0032] Figure 6 This is a comparison chart of the conductive performance of optical fiber carriers;

[0033] Figure 7 and Figure 8This is a graph showing the test results of the optical fiber in Example 2;

[0034] Description of the accompanying drawings: 1. Fiber carrier; 2. Fiber groove; 3. Fiber to be tested; 4. Fiber core; 5. Conductive tape. DETAILED DESCRIPTION

[0035] All features disclosed in this specification, or all steps in the disclosed methods or processes, except mutually exclusive features and / or steps, can be combined in any manner.

[0036] Any feature disclosed in this specification (including any appended claims and abstract), unless otherwise stated, may be replaced by other equivalent or similar features. That is, unless otherwise stated, each feature is only an example of a series of equivalent or similar features.

[0037] In the description of the present invention, it should be understood that the terms "up", "down", "left", "right", etc., indicating directions or positional relationships, are based on the directions or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific direction, be constructed and operated in a specific direction, and therefore cannot be understood as a limitation on the present invention.

[0038] Furthermore, the terms "first," "second," etc., are used for descriptive purposes only and should not be understood to indicate or imply relative importance or to implicitly indicate the quantity of the technical features being referred to. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of such features.

[0039] Example 1

[0040] like Figures 1 to 5 As shown, the present invention provides a technical solution:

[0041] A method for preparing a quartz optical fiber sample for electronic probe testing includes a fiber carrier 1 provided with a fiber groove 2 matching a fiber 3 to be tested; the method includes at least but not limited to the following steps:

[0042] Step 1: First, determine the diameter of the optical fiber 3 to be tested. If the diameter of the optical fiber is not greater than 130μm, use a communication optical fiber cutter to cut it. If the diameter of the optical fiber is greater than 130μm, use a conventional large-core optical fiber cutter to cut it. Use the cutting tool to cut the optical fiber 3 to be tested, and the optical fiber cutting angle is not greater than 1.5°.

[0043] Step 2: Select a fiber optic carrier 1 that matches the diameter of the optical fiber 3 to be tested, and transfer the cut optical fiber 3 to be tested to the optical fiber groove 2 that matches the optical fiber carrier 1. When placing the optical fiber 3 to be tested, the cut end face of the optical fiber 3 to be tested protrudes from the end face of the optical fiber carrier 1.

[0044] Step 3: Push the optical fiber 3 to be tested from its cut end face so that the cut end face of the optical fiber 3 to be tested is flush with the upper end face of the optical fiber carrier 1. During the process of pushing the optical fiber 3 to be tested, contact the optical fiber 3 to be tested along the cut surface or circumferential position of the optical fiber 3 to be tested, and apply force to make the optical fiber 3 to be tested along the end face direction of the optical fiber groove 2 so that the cut end face of the optical fiber 3 to be tested is flush with the upper end face of the optical fiber carrier 1.

[0045] When contacting the optical fiber 3 along the cross-section of the optical fiber 3 to be tested, avoid direct contact with the core 4 of the optical fiber 3 to be tested. This can prevent the optical fiber core in the analyzed area at the geometric center of the optical fiber 3 to be tested from being contaminated, which would have an adverse effect on the experimental test results.

[0046] Step 4: Apply conductive tape across the entire end face of the fiber carrier 1, where the optical fibers 3 to be tested are mounted, to secure all the optical fibers 3 to be tested. The conductive tape should be applied below the end face of the fiber carrier 1. Specifically, the conductive tape should be positioned 0 mm to 2 mm below the end face of the fiber carrier 1. While securing the optical fibers to be tested, manually push the conductive tape to ensure close contact.

[0047] Step 5: Place the optical fiber carrier 1 with the optical fiber attached thereto into a vacuum carbon coating apparatus for carbon coating. The carbon coating thickness is about 20 nm. During the carbon coating process, the upper end surface of the optical fiber carrier faces the carbon end.

[0048] The bottom of the optical fiber groove 2 is a semicircle that matches the curvature of the optical fiber 3 to be tested. When the optical fiber 3 to be tested is placed in the optical fiber groove 2, the optical fiber 3 to be tested fits the bottom of the optical fiber groove 2, thereby ensuring good conductivity.

[0049] The depth of the fiber groove 2 should be at least 50% to 80% of the fiber diameter. This ensures that when the optical fiber 3 to be tested is placed in the optical fiber groove 2, at least half of the optical fiber 3 to be tested is set in the optical fiber groove 2, while also protruding a certain distance from the plane of the optical fiber carrier 1.

[0050] If the diameter of the optical fiber groove 2 is too small, the optical fiber 3 to be tested cannot be effectively fixed. If the diameter of the optical fiber groove 2 is too large, the conductive tape 5 cannot be used to cover and fix the optical fiber.

[0051] The optical fiber carrier 1 in this embodiment is made of a material with good electrical conductivity such as copper or brass.

[0052] The upper and lower surfaces of the optical fiber carrier 1 are parallel. The cross-section of the optical fiber carrier 1 can be square or rectangular.

[0053] In this embodiment, the length of the optical fiber carrier 1 is no more than 30 mm, and the height is no more than 30 mm, so that the optical fiber carrier 1 can be placed in the groove of the electron probe sample stage.

[0054] A plurality of optical fiber grooves 2 can be evenly arranged on the optical fiber carrier 1 as required, and each optical fiber groove 2 is arranged perpendicular to the upper and lower surfaces of the optical fiber carrier 1 .

[0055] This method can significantly shorten the time required to prepare one or more samples. The optical fiber sample preparation process, including cutting, mounting on the optical fiber carrier 1, and carbon coating, takes no more than two hours. Unlike traditional sample preparation methods, the cutting and mounting processes take no more than 10 minutes.

[0056] The fiber cross-sectional information obtained through this solution is accurate. Because the fiber cutting angle is no greater than 1.5 degrees, the cut end face is the fiber cross-section, not the beveled surface. Therefore, the cross-sectional information of the fiber sample prepared by this technical solution (such as the fiber core diameter and the circularity of the fiber core) is accurate.

[0057] In this solution, since the optical fiber is installed in the optical fiber groove 2 which is perpendicular to the optical fiber carrier 1, the optical fiber analysis surface is horizontal and the test effect is good. Figure 4 The optical microscope focusing diagram of the electron probe after sample preparation using the prior art is shown as follows: Figure 5 The optical microscope focus image of the electron probe after the sample was prepared using this method is shown in the figure. Figure 4 The optical microscope focus of the electron probe failed and the sample surface was not level. Figure 5 The sample surface is level and in focus.

[0058] At the same time, since the optical fiber analysis surface is flush with the upper surface of the optical fiber carrier 1 and is coated with the conductive tape 5, the optical fiber carrier 1 has good conductivity. Therefore, the optical fiber sample after carbon spraying has good conductivity. Figure 6 Conductive performance comparison chart.

[0059] Example 2

[0060] This embodiment adopts the method of the above embodiment 1 to test the doping composition of the YbAlP-doped silica optical fiber with a core diameter of 20 microns and an optical fiber diameter of 400 microns. The test results are as follows: Figure 7 and Figure 8 shown.

[0061] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A method for preparing a quartz optical fiber sample for electron probe testing, characterized in that: The optical fiber carrier includes an optical fiber groove having a size matching that of the optical fiber to be tested. The preparation method includes the following steps: Step 1: Select an appropriate cleaver according to the diameter of the optical fiber to be tested and cut the optical fiber to be tested. The cutting angle should not exceed 1.5°. Step 2: Transfer the cleaved optical fiber to be tested to the optical fiber groove of the optical fiber carrier that matches it. When placing the optical fiber to be tested, the cleaved end face of the optical fiber to be tested protrudes from the end face of the optical fiber carrier. Step 3: Push the optical fiber to be tested from its cleaved end face so that the cleaved end face of the optical fiber to be tested is flush with the upper end face of the optical fiber carrier; Step 4: Use conductive tape to stick across the entire end face of the optical fiber carrier where the optical fiber to be tested is set, and tighten all the optical fibers to be tested. The sticking position of the conductive tape is lower than the end face of the optical fiber carrier; Step 5: Place the optical fiber carrier with the optical fiber attached into a vacuum carbon coating apparatus for carbon coating. During the carbon coating process, the upper end surface of the optical fiber carrier faces the carbon end.

2. The method for preparing a quartz optical fiber sample for electron probe testing according to claim 1, wherein: In step 1, when judging the diameter of the optical fiber to be tested, if the diameter of the optical fiber is not greater than 130 μm, a communication optical fiber cutter is used for cutting; if the diameter of the optical fiber is greater than 130 μm, a large-diameter optical fiber cutter is used for cutting. The optical fiber to be tested is cut using a cutting tool.

3. The method for preparing a quartz optical fiber sample for electron probe testing according to claim 2, wherein: In step three, while pushing the optical fiber to be tested, the optical fiber to be tested is contacted along the cut surface or circumferential position of the optical fiber to be tested, and a force is applied along the length direction of the optical fiber groove to make the cut end surface of the optical fiber to be tested flush with the upper end surface of the optical fiber carrier.

4. The method for preparing a quartz optical fiber sample for electron probe testing according to claim 3, wherein: In step 4, the conductive tape is 0 mm to 2 mm lower than the end surface of the optical fiber carrier.

5. A method for preparing a quartz optical fiber sample for electron probe testing according to any one of claims 1 to 4, characterized in that: The bottom of the optical fiber groove is a semicircle that matches the curvature of the optical fiber to be tested. When the optical fiber to be tested is placed in the optical fiber groove, the optical fiber to be tested fits the bottom of the optical fiber groove. The depth of the optical fiber groove should be at least 50% to 80% of the optical fiber diameter.

6. A method for preparing a quartz optical fiber sample for electron probe testing according to any one of claims 1 to 4, characterized in that: The optical fiber carrier is made of a non-magnetic metal material with good electrical conductivity.

7. A method for preparing a quartz optical fiber sample for electron probe testing according to any one of claims 1 to 4, characterized in that: The upper and lower surfaces of the optical fiber carrier are parallel, and the cross-section of the optical fiber carrier is square or rectangular.

8. The method for preparing a quartz optical fiber sample for electron probe testing according to any one of claims 1 to 4, characterized in that: The length of the optical fiber carrier is no more than 30 mm, and the height is no more than 30 mm.

9. The method for preparing a quartz optical fiber sample for electron probe testing according to any one of claims 1 to 4, characterized in that: A plurality of optical fiber grooves are evenly arranged on the optical fiber carrier, and each optical fiber groove is arranged perpendicular to the upper and lower surfaces of the optical fiber carrier.

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