Optical fiber component testing method based on electronic probe

Abstract

The invention discloses an optical fiber component testing method based on an electronic probe, and relates to the field of quartz material testing, and the method comprises the following steps: carrying out carbon plating treatment on a to-be-tested optical fiber sample; performing line scanning test on the carbon-plated optical fiber sample to be tested by adopting an electronic probe to obtain line scanning analysis data of each element to be tested; carrying out quantitative analysis test on the carbon-plated optical fiber sample to be tested by adopting an electronic probe to obtain quantitative analysis data of each element to be tested; and determining the component distribution of the optical fiber sample to be detected according to the line scanning analysis data of each element to be detected and the quantitative analysis data of each element to be detected. By combining line scanning and quantitative analysis of the electronic probe, the test precision of the optical fiber components is improved.

Description

Technical Field

[0001] The present application relates to the field of quartz material testing, and in particular to an optical fiber component testing method based on an electronic probe. Background Art

[0002] Optical fiber materials are generally divided into two types: active and passive. Active optical fiber is generally doped with rare earth elements. Rare earth-doped gain fiber is an important component of fiber lasers, which can greatly determine the output quality of the laser. At present, the doped rare earth particles in quartz optical fiber mainly include erbium (Er), neodymium (Nd), ytterbium (Yb), thulium (Tm), holmium (Ho), etc. Among them, Yb 3+ Ion fiber lasers have the highest light conversion efficiency. The main research direction of Ytterbium Doped Fiber (YDF) is to adjust the cladding refractive index of the fiber core and obtain a higher rare earth ion doping concentration. Passive optical fiber is mainly germanium-doped fiber, which is mainly used for energy transmission fiber and communication fiber of fiber lasers. However, due to the small size of the optical fiber, which is often only about 10μm, a more precise preparation process is required.

[0003] Therefore, during the optical fiber preparation process, it is necessary to precisely control the composition of the optical fiber core and optimize the preparation process to obtain an ideal optical structure and excellent output performance. Summary of the invention

[0004] The purpose of this application is to provide an optical fiber component testing method based on an electronic probe, which can improve the accuracy of optical fiber component testing.

[0005] To achieve the above objectives, this application provides the following solutions:

[0006] The present application provides a method for testing optical fiber components based on an electronic probe, comprising:

[0007] Carry out carbon coating treatment on the optical fiber sample to be tested;

[0008] The electronic probe is used to perform line scanning test on the carbon-plated optical fiber sample to obtain the line scanning analysis data of each element to be tested;

[0009] The carbon-plated optical fiber samples were quantitatively analyzed by electron probe to obtain quantitative analysis data of each element to be tested.

[0010] The component distribution of the optical fiber sample to be tested is determined based on the line scanning analysis data of each element to be tested and the quantitative analysis data of each element to be tested.

[0011] According to the specific embodiments provided in this application, this application has the following technical effects:

[0012] The present application provides an optical fiber component testing method based on an electronic probe. By combining the line scanning and quantitative analysis of the electronic probe, line scanning testing and quantitative analysis testing are performed on the optical fiber sample to be tested. Low-content elements can be accurately analyzed, and the component distribution of the optical fiber sample to be tested is determined based on the line scanning analysis data of each element to be tested and the quantitative analysis data of each element to be tested, thereby improving the testing accuracy of the optical fiber components. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0014] Figure 1 A schematic diagram of a process flow of an optical fiber component testing method based on an electronic probe provided in one embodiment of the present application;

[0015] Figure 2 A schematic diagram of optical fiber cutting in one embodiment of the present application;

[0016] Figure 3 This is a backscattering image of sample 1 in one embodiment of the present application;

[0017] Figure 4 This is a COMPO diagram of sample 1 in one embodiment of the present application;

[0018] Figure 5 This is a spectrometer component distribution diagram of sample 1 in one embodiment of the present application;

[0019] Figure 6 This is an electron probe line scan and quantitative analysis fitting curve diagram of sample 1 in one embodiment of the present application;

[0020] Figure 7 This is a fitting curve diagram of the electron probe line scan and quantitative analysis of sample 2 in one embodiment of the present application.

[0021] Reference numerals: 201 - optical fiber cutting knife, 202 - cutting surface. DETAILED DESCRIPTION

[0022] The following will be combined with the drawings in the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0023] The traditional optical fiber structure generally includes a core, a cladding, and a coating. The size of the optical fiber is relatively small, and is generally divided into fixed sizes such as 10 / 125 and 20 / 400, and the core size is only 10μm-20μm. Due to the small size of the optical fiber core, the micro-area analysis method is the best choice for its component analysis, such as the use of a scanning electron microscope (Scanning Electron Microscope, SEM) energy dispersive spectrometer (Energy Dispersive Spectrometer, EDS) or an electron probe (Electron Probe Micro-Analysis, EPMA) spectrometer (Wavelength Dispersive Spectrometer, WDS). Both EPMA and SEM use a focused electron beam to irradiate the surface of the sample being tested, and use WDS or EDS to detect the characteristic X-ray wavelength and signal strength generated by the interaction between electrons and samples, so as to perform qualitative or quantitative analysis on the elements contained in the micro-area.

[0024] Traditional EDS analysis and testing is mainly used for large metal compound materials. The test electron beam current is relatively large (5μm-10μm), and the test accuracy is very limited, which cannot meet the current process requirements of optical fibers. In addition, the traditional SEM-EDS backscatter image cannot determine the exact position of the fiber core, let alone accurately test the fiber core, and the analysis of elements is very limited. When facing inorganic silicate materials such as optical fibers, the Mass% (mass percentage) of the overall SiO2 is 80%-100%, and the Mass% of various doping elements is only 4%-5%. The concentration of the components varies greatly, and the testing difficulty is therefore higher. Therefore, SEM-EDS cannot reflect the linear component fluctuations of the doping elements, and it is difficult to meet the preparation / detection process requirements of optical fibers.

[0025] EPMA can be used for surface morphology observation and micro-area composition analysis of samples, and is widely used in qualitative analysis, quantitative analysis and line scanning of materials. EPMA has a sufficiently large and stable electron beam current, a high peak-to-background ratio, and a wide range of element measurement including ultra-light elements. Compared with traditional SEM-EDS analysis, it can obtain high-sensitivity and high-resolution backscattered electron images, presenting micro-phase distribution phenomena at the micron level, which is very conducive to precise positioning and accurate analysis of the analysis area.

[0026] EPMA's line scanning analysis mainly uses a very small electron beam (<2μm) to bombard the sample to be tested. During the test, the characteristic X-ray signal generated by the electrons and the material is compared. This method is mainly used for qualitative analysis and cannot accurately determine the specific content of each element in the sample, nor can it accurately control the doping content in the preparation process. At the same time, EPMA's quantitative analysis uses a specific size of electron beam to bombard the sample surface to determine the specific content of the element. In order to ensure accuracy, the electron beam spot is required to be larger (1μm-2μm), but the fiber core is only 10μm-20μm. The sample test can only produce a very small amount of path information, and the test accuracy cannot meet the results required by the process.

[0027] This application utilizes the unique high-resolution advantage of EPMA, combines qualitative line scanning and quantitative analysis, and accurately analyzes the doping composition of optical fibers, providing strong support for improving optical fiber preparation processes and material ratios.

[0028] In order to make the above-mentioned objects, features and advantages of the present application more obvious and easy to understand, the present application is further described in detail below in conjunction with the accompanying drawings and specific implementation methods.

[0029] In an exemplary embodiment, Figure 1 As shown, a method for testing optical fiber components based on an electronic probe is provided, including the following steps 101 to 105.

[0030] Step 101, remove the coating layer of the optical fiber sample to be tested, and longitudinally cut the optical fiber sample to be tested; use conductive glue to vertically fix the longitudinally cut optical fiber sample to be tested on a sample table, so that the cut surface of the optical fiber sample to be tested is upward and flush with the sample table, and the cut surface of the optical fiber sample to be tested is higher than the set height of the conductive glue.

[0031] The optical fiber sample to be tested is an active optical fiber or a passive optical fiber.

[0032] Specifically, remove the coating layer of the optical fiber sample to be tested, wipe the surface clean with alcohol to prevent contamination by oil, dust and water stains. Figure 2 As shown, the optical fiber sample to be tested is cut longitudinally using an optical fiber cutting knife 201 to obtain a flat cut surface 202, and then the optical fiber sample to be tested after the longitudinal cut is fixed vertically on the sample stage using conductive glue, so that the cut surface 202 of the optical fiber sample to be tested faces upward and the end of the sample stage is flush, and then it is fixed again using conductive glue to ensure that the cut surface 202 of the optical fiber sample to be tested is 0.5mm higher than the conductive glue, which can ensure that the cut surface 202 of the optical fiber after carbon coating has a good conductive effect and prevent the electronic signal generated in the test from being blocked by the conductive glue.

[0033] Step 102, performing carbon coating treatment on the optical fiber sample to be tested.

[0034] In a specific application example, a vacuum carbon coating machine is used to perform carbon coating on the optical fiber sample to be tested. During the carbon coating process, the vacuum degree of the carbon coating chamber of the vacuum carbon coating machine is less than 10 -3 pa.

[0035] Since the optical fiber is made of inorganic silicate materials, the material itself is not conductive, so it needs to be carbon-plated to obtain good test results. Specifically, place the sample table on the rotating table of the vacuum carbon coating machine and pump the vacuum degree of the carbon coating chamber to 10 -3 The carbon rod is sputtered below pa, so that the surface of the cut surface 202 of the optical fiber sample to be tested has a uniform carbon film with a suitable thickness. The thickness of the carbon film is 20nm.

[0036] Step 103, use an electronic probe to perform a line scan test on the carbon-plated optical fiber sample to obtain line scan analysis data of each element to be tested. The line scan analysis data includes position information and component content information.

[0037] In a specific application example, step 103 includes the following steps 31 to 34.

[0038] Step 31, determine the test conditions of the line scan test. The test conditions of the line scan test are: voltage is 15KV, current is 50nA, line scan length is 1.5 times the core length of the carbon-plated optical fiber sample to be tested, relaxation time is 500ms, electron beam spot is 0.1μm, and the number of dots = scan length / electron beam spot.

[0039] Specifically, adjust the carbon-coated fiber sample to the center of the EPMA view, zoom in to a suitable size, select the COMPO view mode, and adjust the brightness and contrast until the electronic morphology of the fiber core can be clearly seen. Then select the line scan program corresponding to each element to be tested, determine the test conditions, and ensure that the two segments of the line scan and the center position are well focused.

[0040] Step 32, select several elements to be tested and the test channels corresponding to each element to be tested. Specifically, the corresponding test channel is selected according to the characteristic lattice of each element to be tested.

[0041] Step 33, based on the test conditions of the line scan test, each element to be tested and the test channel corresponding to each element to be tested, a line scan test is performed on the carbon-plated optical fiber sample to be tested, and a peak is searched at a focusing position outside the line scan path and within the core of the carbon-plated optical fiber sample to be tested to obtain the peak spectrum value of each element to be tested.

[0042] Step 34, determining the line scan analysis data of each element to be detected according to the peak spectrum value of each element to be detected.

[0043] Step 104: Use an electronic probe to perform quantitative analysis on the carbon-plated optical fiber sample to obtain quantitative analysis data of each element to be tested. The quantitative analysis data includes position information and component content information.

[0044] In a specific application example, step 104 includes the following steps 41 to 44 .

[0045] Step 41, determine the test conditions for the quantitative analysis test. The test conditions for the quantitative analysis test are: voltage is 15KV, current is 10nA, scanning length is 1.2 times the core length of the carbon-plated optical fiber sample to be tested, electron beam spot is 2μm, and the number of dots = scanning length / electron beam spot.

[0046] Specifically, adjust the carbon-coated fiber sample to the center of the EPMA view, zoom in to a suitable size, select the COMPO view mode, and adjust the brightness and contrast until the backscattered electron morphology of the fiber core can be clearly seen. Then select the quantitative analysis program corresponding to each element to be tested, determine the test conditions, and ensure that each position of the quantitative analysis is well focused.

[0047] Step 42, select several elements to be tested and the test channels corresponding to each element to be tested. Specifically, the corresponding test channel is selected according to the characteristic lattice of each element to be tested.

[0048] Step 43, based on the test conditions of the quantitative analysis test, each element to be tested and the test channel corresponding to each element to be tested, a quantitative analysis test is performed on the carbon-plated optical fiber sample to be tested, and a peak is searched at a focusing position outside the online scanning path and within the core of the carbon-plated optical fiber sample to be tested to obtain the peak spectrum value of each element to be tested.

[0049] Step 44, determining the quantitative analysis data of each element to be measured according to the peak spectrum value of each element to be measured.

[0050] Line scan analysis data and quantitative analysis data can be directly output as TXT text through the electron probe. This application mainly focuses on the position information and component content information therein.

[0051] Step 105, determining the component distribution of the optical fiber sample to be tested according to the line scan analysis data of each element to be tested and the quantitative analysis data of each element to be tested.

[0052] In a specific application example, in step 105, the line scan analysis data and the quantitative analysis data are fitted using data analysis software (such as origin) to accurately test the specific component distribution of the optical fiber sample to be tested. First, the line scan analysis data and the quantitative analysis data in TXT format are converted into EXCEL format, and the position information and component content information are respectively inserted into the data analysis software, and the corresponding names, units and comments are set. Step 105 includes the following steps 51 to 54.

[0053] Step 51, according to the core size of the optical fiber sample to be tested after carbon coating and the test step length of the line scanning test, position normalization processing is performed on the line scanning analysis data of each element to be tested to obtain a preliminary line scanning curve.

[0054] Specifically, the fiber core size is determined according to the test coordinate information, the median of the coordinate information is set as the center 0 point, and the remaining position information is distributed around the 0 point according to the test step of the line scan test to obtain a preliminary line scan curve. The preliminary line scan curve is a broken line graph.

[0055] Step 52, according to the core size of the optical fiber sample to be tested after carbon coating and the test step length of the quantitative analysis test, the quantitative analysis data of each element to be tested is positionally normalized to obtain a preliminary quantitative analysis curve.

[0056] Specifically, the fiber core size is determined according to the test coordinate information, the median of the coordinate information is set as the center 0 point, and the remaining position information is distributed around the 0 point according to the test step of the quantitative analysis test to obtain a preliminary quantitative analysis curve. The preliminary quantitative analysis curve is a point-line graph.

[0057] Step 53 , respectively performing component normalization processing on the preliminary line scan curve and the preliminary quantitative analysis curve, setting the extreme value points of the preliminary line scan curve and the preliminary quantitative analysis curve on the same standard line, and obtaining a final line scan curve and a final quantitative analysis curve.

[0058] Specifically, the reference points at both ends of the preliminary line scan curve and the preliminary quantitative analysis curve are selected. According to the component test requirements, the test range must cover the entire core diameter, so the reference point of the doping element is the lowest point with a content of 0%, and the reference point of the matrix Si element is the content of 100%. The reference points of the preliminary line scan curve and the preliminary quantitative analysis curve are set on the same reference line. Then select the core extreme points of the preliminary line scan curve and the preliminary quantitative analysis curve. The extreme point of the doping element is the highest content point, and the extreme point of the matrix Si element is the lowest content point. Further adjust the coordinate ratio of the final line scan curve and the final quantitative analysis curve so that the final line scan curve and the final quantitative analysis curve are of appropriate size.

[0059] Step 54, determining the content of each element at each position of the optical fiber sample to be tested according to the final line scan curve and the final quantitative analysis curve, so as to determine the component distribution of the optical fiber sample to be tested.

[0060] In an exemplary embodiment, the peak search process in step 43 and step 53 is further adjusted according to predetermined standard sample information of each element to be measured. The standard sample information is the signal amount of each element to be measured when the content is 100%.

[0061] Since optical fibers produced by different equipment have slight differences in internal structure and composition, which leads to inaccurate testing, the present application can make the test more accurate by pre-testing standard samples of optical fibers obtained by different production methods.

[0062] The process of determining the standard sample information of each element to be measured includes: placing a number of standard samples corresponding to the elements to be measured into the sample chamber of the EPMA, evacuating the chamber to 10 -4 Below pa, turn on the tungsten filament, select the standard sample to be tested and the corresponding STD standard sample program, set the voltage to 15KV, the current to 10nA, select 3 well-focused positions on the standard sample, and enter the position information into the program. Select the standard sample elements (such as Yb, P, Al, Si, Ge, Er, F elements) and their corresponding test channels, and select any well-focused position outside the path for peak search. After peak search, read the peak position into the program, start the test, and obtain the standard sample information of the element to be tested. According to the above steps, test the standard samples corresponding to different elements to be tested in turn to obtain some standard sample information corresponding to the elements to be tested.

[0063] Different from traditional EDS component analysis test, single qualitative analysis or single quantitative analysis, this application adopts a combination of EPMA and qualitative and quantitative methods to accurately test the component information of optical fiber. Compared with traditional detection and analysis methods, the method provided by this application has the following advantages:

[0064] (1) Compared with traditional EDS, the spectral peak of EPMA-WDS is narrower and the peak-to-background ratio is relatively high, so the detector sensitivity is higher, especially for the analysis of low-content elements, which is significantly better than EDS. In addition, WDS has high energy resolution and can eliminate the interference of a large number of L, M and N series spectral lines of superheavy elements near the K line of ultralight elements. Although the calculation of the spectral line overlap coefficient after the M series is more difficult, and the background in the low-energy region is also difficult to estimate, so the analysis of low-content and ultra-light elements is more difficult, but the present application can accurately analyze low-content elements using the EPMA-WDS method.

[0065] (2) The principle of elemental analysis using EPMA-WDS in this application is to set the spectrometer at the characteristic X-ray wavelength position of a certain element to be analyzed, use the electron beam scanning accessory or the sample stage to move the electron beam to scan the specified area, and record the X-ray intensity point by point to obtain the distribution of the element in the specified area. WDS can distinguish the characteristic X-ray energy between elements with low content or small concentration differences, so it can well show the distribution differences of elements.

[0066] (3) The present application uses the COMPO image of the electron probe to clearly display the morphology of the fiber core, better locate the position of the fiber core, and accurately analyze the elemental composition. When EDS is tested, only points can be manually selected for testing in batches, resulting in very rough composition information, while EPMA can automatically generate a test path based on the location information of the sample, set the program for automatic testing according to the range of the sample to be tested, and conveniently and accurately provide information on the distribution of sample surface components.

[0067] In order to verify the accuracy of the fiber component test of this application, the EPMA and EDS component analysis data of the quartz optical fiber are analyzed and compared. Two test samples are prepared: sample 1 and sample 2. The application method is demonstrated through the application environment of active optical fiber and passive optical fiber respectively. The core diameter of sample 1 is 16μm and the cladding diameter is 125μm; the core diameter of sample 2 is 20μm and the cladding diameter is 400μm. The comparative analysis process is as follows.

[0068] (1) Prepare the sample to be tested.

[0069] Remove the coating layer of sample 1, wipe the surface with alcohol, and use the fiber cleaver 201 to cut the fiber longitudinally to obtain a flat cut surface 202. Then use conductive glue to fix the non-cut surface end of sample 1 vertically on the sample stage, with the cut surface 202 facing upward and parallel to the sample stage. Place the sample stage in a vacuum carbon coating machine and draw the vacuum degree of the carbon coating chamber to 10 -3 The carbon rod is sputtered below pa, so that the surface of the cut surface 202 of the optical fiber has a uniform carbon film with a suitable thickness. The vacuum degree is 8×10 -3 pa, the sputtering current is 22A, the sputtering time is 40s, and the carbon film thickness is 20nm.

[0070] (2) Prepare standard sample information.

[0071] EPMA was used to perform component testing. Standard samples corresponding to the elements to be tested were placed in the sample chamber. The elements to be tested and the standard samples in this embodiment are shown in Table 1. The chamber was evacuated to 10 -4Below pa, turn on the tungsten filament, select the standard sample to be tested and the corresponding STD standard sample program, set the voltage to 15KV, the current to 10nA, select 3 well-focused positions on the standard sample, and enter the position information into the program. Select the elements to be tested Yb, P, Al, Si, Ge, Er, and F respectively, select the corresponding test channels according to the characteristic crystals of different elements, and select any well-focused position outside the path for peak search. After peak search, read the spectrum peak position into the program, and start testing each element to be tested in turn.

[0072] Table 1 Standard sample information

[0073] element Al P Si Yb Er Ge F Standard <![CDATA[Al2O3]]> <![CDATA[YbPO4]]> <![CDATA[SiO2]]> <![CDATA[YbPO4]]> <![CDATA[ErPO4]]> <![CDATA[Bi4Ge3O 12 ]]> <![CDATA[Al2SiO4(F,OH)2]]> Crystal TAP PETJ TAP LIFH LDE1 TAP TAP

[0074] (3) Use SEM-EDS to conduct composition analysis test.

[0075] Place the sample to be tested into the sample chamber of the scanning electron microscope, enlarge it to a suitable size, select the backscattering mode, and the test results are as follows: Figure 3 As shown, it can be seen that EDS cannot accurately locate the position of the fiber core. The experiment can only use geometric position to select a 100μm square block in the middle of the optical fiber for rough testing. The voltage is set to 15KV, the electron beam spot is set to 3μm, and the corresponding elements are selected for analysis and testing. Figure 4 This is the COMPO image test result, which also reflects the inaccuracy of EDS testing. The fluctuations of the components inside the fiber core cannot be reflected, which does not meet the requirements of process preparation testing.

[0076] (4) Use EPMA to perform component analysis test.

[0077] First, use EPMA to perform line scanning qualitative testing. Place the sample to be tested in the sample chamber of EPMA, adjust the sample to the center, enlarge it to a suitable size, select COMPO image mode, and the test results are as follows: Figure 5 As shown. Due to the contrast of each element, the morphology of the fiber core can be clearly seen, which is convenient for positioning, the test range is reduced, and the test accuracy is higher. Select the line scan program, set the voltage to 15KV, adjust the current to 50nA, determine the line scan length to 30μm according to the core size, the relaxation time to 500ms, the electron beam spot to 0.1μm, the number of dots to 300, and confirm the program. Then use EPMA for quantitative analysis and testing. Select the quantitative analysis program, set the voltage to 15KV, adjust the current to 10nA, determine the quantitative analysis length to 30μm according to the core size, select the electron beam spot to 2μm, the number of dots to 15, confirm the program, and start the analysis and test.

[0078] (5) Use data analysis software to fit and analyze the data.

[0079] The quantitative analysis data and line scanning analysis data of each element to be measured obtained in step (3) and step (4) are converted from TXT format to EXCEL format, and the position information and component content information of each element to be measured are respectively inserted into the data analysis software, and the corresponding names, units, and comments are set.

[0080] The line scan analysis data and the quantitative analysis data are sequentially subjected to position normalization processing and component normalization processing to generate line scan curves and quantitative analysis curves, and a suitable coordinate scale is set to adjust the line scan curves and the quantitative analysis curves to a suitable size for data analysis.

[0081] It can be clearly seen from the line scan curve and quantitative analysis curve that in EDS testing, the approximate location of the core can only be identified by the agglomeration of elements, and the core position cannot be accurately located, thereby expanding the test range and reducing the sensitivity of the components. In addition, due to the large electron beam spot of the EDS test and limited resolution, the concentration difference distribution of the components cannot be effectively displayed.

[0082] This application uses a combination of line scanning and quantitative analysis to accurately analyze the specific component distribution of the optical fiber core, and the results are as follows: Figure 6 As shown, we can clearly see the component distribution of the active optical fiber of sample 1. Sample 1 contains elements such as Al, Ge, P, Si, Er, and Yb. By combining line scanning with quantitative analysis, we can see that since the Al and Ge elements are distributed in annular shapes, the Al and Ge rings are narrow and only 4μm thick. The quantitative analysis can only cover 2 test points at most, but line scanning can cover 40 test points, which clearly reflects the concentration changes of the elements. Combined with the values ​​of quantitative analysis, the values ​​of each micro-test point can be analyzed, and the concentration distribution of the core elements can be more clearly shown. At the same time, it can be seen from the distribution of rare earth elements Er and Yb that even if the element doping amount is only 0mass%-0.26mass%, the fluctuation of the composition can be clearly reflected, which reflects the precise test performance of EPMA and the reliability of the test method combining EPMA line scanning and quantitative analysis.

[0083] Sample 2 was tested and analyzed using the same method as above. The test results are as follows: Figure 7As shown, F is a light element, and it is difficult to accurately measure the specific content of F in the material through general EDS testing. The optical fiber component testing method provided in this application can clearly show the specific content, even if the maximum content of F element is only 0.3 mass%. By combining line scanning with quantitative analysis, the distribution of F element inside the material can be clearly analyzed. Similarly, the Ge element is distributed in a ring shape inside the material, with a ring width of 5μm. Only two values ​​can be analyzed through quantitative analysis, but combined with line scanning, it can be found that there is a 2μm platform at the highest Ge element content. Secondly, the stability of this application can be seen from the Al element, and there is no obvious test error.

[0084] It should be noted that the user information (including but not limited to user device information, user personal information, etc.) and data (including but not limited to data used for analysis, stored data, displayed data, etc.) involved in this application are all information and data authorized by the user or fully authorized by all parties, and the collection, use and processing of relevant data must comply with relevant regulations.

[0085] In this application, all actions to obtain signals, information or data are carried out in compliance with the relevant data protection laws and policies of the country where they are located and with the authorization given by the owner of the corresponding device.

[0086] The technical features of the above embodiments may be arbitrarily combined. To make the description concise, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0087] This article uses specific examples to illustrate the principles and implementation methods of this application. The description of the above embodiments is only used to help understand the method and core ideas of this application. At the same time, for those skilled in the art, according to the ideas of this application, there will be changes in the specific implementation methods and application scope. In summary, the content of this specification should not be understood as limiting this application.

Claims

1. A method for testing optical fiber components based on an electronic probe, characterized in that: The optical fiber component testing method based on electronic probe includes: Carry out carbon coating treatment on the optical fiber sample to be tested; The electronic probe is used to perform line scanning test on the carbon-plated optical fiber sample to obtain the line scanning analysis data of each element to be tested; The carbon-plated optical fiber samples were quantitatively analyzed by electron probe to obtain quantitative analysis data of each element to be tested. The component distribution of the optical fiber sample to be tested is determined based on the line scanning analysis data of each element to be tested and the quantitative analysis data of each element to be tested.

2. The optical fiber component testing method based on electronic probe according to claim 1, characterized in that: Before the optical fiber sample to be tested is subjected to carbon plating, the optical fiber component testing method based on an electronic probe further comprises: Removing the coating layer of the optical fiber sample to be tested, and longitudinally cutting the optical fiber sample to be tested; The longitudinally cut optical fiber sample to be tested is fixed vertically on the sample stage with conductive glue, so that the cut surface of the optical fiber sample to be tested faces upward and is flush with the sample stage, and the cut surface of the optical fiber sample to be tested is higher than the height set by the conductive glue.

3. The optical fiber component testing method based on electronic probe according to claim 1, characterized in that: The optical fiber sample to be tested is subjected to carbon coating treatment, which specifically includes: A vacuum carbon coating machine is used to coat the optical fiber sample to be tested. During the carbon coating process, the vacuum degree of the carbon coating chamber of the vacuum carbon coating machine is less than 10 -3 pa.

4. The optical fiber component testing method based on electronic probe according to claim 1, characterized in that: The carbon-plated optical fiber sample was subjected to line scanning test using an electron probe to obtain line scanning analysis data for each element to be tested, including: Determine test conditions for line scan testing; Select several elements to be tested and the test channels corresponding to each element to be tested; Based on the test conditions of the line scan test, each element to be tested and the test channel corresponding to each element to be tested, a line scan test is performed on the carbon-plated optical fiber sample to be tested, and a peak is searched at a focusing position outside the line scan path and within the core of the carbon-plated optical fiber sample to be tested to obtain a peak spectrum value of each element to be tested; According to the peak spectrum value of each element to be measured, the line scan analysis data of each element to be measured is determined.

5. The optical fiber component testing method based on electronic probe according to claim 4, characterized in that: The test conditions of the line scan test are: voltage of 15KV, current of 50nA, line scan length of 1.5 times the core length of the carbon-plated optical fiber sample to be tested, relaxation time of 500ms, and electron beam spot of 0.1μm.

6. The optical fiber component testing method based on electronic probe according to claim 1, characterized in that: The carbon-plated optical fiber samples were quantitatively analyzed by electron probe to obtain quantitative analysis data of each element to be tested, including: Determine test conditions for quantitative analytical tests; Select several elements to be tested and the test channels corresponding to each element to be tested; Based on the test conditions of the quantitative analysis test, each element to be tested and the test channel corresponding to each element to be tested, the carbon-plated optical fiber sample to be tested is subjected to quantitative analysis test, and the peak is searched at the focusing position outside the line scanning path and within the core of the carbon-plated optical fiber sample to be tested to obtain the peak spectrum value of each element to be tested; According to the peak spectrum value of each element to be measured, the quantitative analysis data of each element to be measured is determined.

7. The optical fiber component testing method based on electronic probe according to claim 6, characterized in that: The test conditions for the quantitative analysis test are: voltage of 15 KV, current of 10 nA, scanning length of 1.2 times the core length of the optical fiber sample to be tested after carbon coating, and electron beam spot of 2 μm.

8. The optical fiber component testing method based on electronic probe according to claim 4 or 6, characterized in that: The optical fiber component testing method based on electronic probe also includes: The peak search process is adjusted according to the predetermined standard sample information of each element to be measured; the standard sample information is the signal amount of each element to be measured when the content is 100%.

9. The optical fiber component testing method based on electronic probe according to claim 1, characterized in that: The line scan analysis data and the quantitative analysis data both include position information and component content information.

10. The optical fiber component testing method based on electronic probe according to claim 1, characterized in that: According to the line scanning analysis data of each element to be tested and the quantitative analysis data of each element to be tested, the component distribution of the optical fiber sample to be tested is determined, including: According to the core size of the optical fiber sample to be tested after carbon coating and the test step length of the line scanning test, the line scanning analysis data of each element to be tested is positionally normalized to obtain a preliminary line scanning curve; According to the core size of the optical fiber sample to be tested after carbon coating and the test step length of the quantitative analysis test, the quantitative analysis data of each element to be tested is positionally normalized to obtain a preliminary quantitative analysis curve; Performing component normalization processing on the preliminary line scanning curve and the preliminary quantitative analysis curve respectively, setting the extreme value points of the preliminary line scanning curve and the preliminary quantitative analysis curve on the same standard line, and obtaining a final line scanning curve and a final quantitative analysis curve; According to the final line scanning curve and the final quantitative analysis curve, the content of each element at each position of the optical fiber sample to be tested is determined to determine the component distribution of the optical fiber sample to be tested.

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