CN111103316B - Calculation method for non-conductive ceramic material non-charge balance voltage - Google Patents
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- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention provides a method for calculating the non-charge balance voltage of a non-conductor ceramic material, which comprises the following steps: setting the optimal working distance of X-ray energy spectrum analysis; the incident acceleration voltage of the scanning electron microscope continuously changes at specified intervals, and an X-ray energy spectrum signal is collected; storing all counting points of the acquired X-ray energy spectrum signals into a TXT format, introducing the counting points into a Matlab program, and calculating the upper limit voltage of the energy spectrum line corresponding to each X-ray energy spectrum signal by adopting linear fitting; and introducing the calculated upper limit voltage into a Matlab program for piecewise linear fitting, and calculating two intersection values of a piecewise fitting curve and a theoretical straight line, wherein the two intersection values are the non-charge balance voltage of the sample to be detected. The method can be directly applied to the observation of the shapes of the scanning electron microscopes of common ceramic samples and other non-conductor materials, and has the advantages of simple operation, accurate result and strong repeatability.
Description
Technical Field
The invention relates to the field of characterization of morphology and components of a scanning electron microscope of a non-conductive ceramic material, in particular to a non-charge balance voltage V of the non-conductive ceramic material1And V2The method of (3).
Background
Scanning Electron Microscopes (SEM) have many advantages such as high image resolution (3 nm-0.6 nm), large depth of field (10 times of that of an optical Electron Microscope), nondestructive analysis, simple sample preparation and the like. The sample can be a natural surface, a fracture, a block, a reflective and transparent light sheet and the like. Meanwhile, the information such as morphology, chemical composition, element distribution and the like can be comprehensively analyzed after accessories such as an Energy Dispersive X-Ray Spectroscopy (EDX) are equipped, and the method becomes one of the most main means for material microstructure characterization.
However, for non-conductor materials, such as most ceramic materials, etc., the incident electrons of the scanning electron microscope form unstable electric fields on the surface and subsurface of the sample due to the accumulation of electric nuclei, so that a "discharge phenomenon" or a "charge phenomenon" occurs, and the morphology and component characterization results are seriously affected. Therefore, when the morphology and the energy spectrum component of the non-conductive ceramic material are analyzed, a layer of conductive C, Cr, Pt film and the like is generally evaporated on the surface of a sample to eliminate the charging phenomenon.
However, the coating method introduces foreign particles on the surface of the sample, and the particles cannot be observed under a scanning electron microscope by 10 ten thousand times, but are obviously shown in an image by more than 10 ten thousand times, so that the real microstructure of the material is hidden. Particularly, with the rapid development of the present nanoscience technology, more and more attention is paid to the details of the surface morphology of the material in the nanometer scale, and the microstructure characteristics of the material in the nanometer scale can be represented only under the magnification of 20 ten thousand times or even higher. Especially for microstructure details only a few nanometers in size, such as mesoporous materials, etc., will severely mask the surface details of the sample after coating. Specifically, fig. 5 shows the charge morphology of lutetium aluminum garnet laser ceramic (LuAG) under 5KV unbalanced voltage, and as shown in fig. 5, bright stripes in the image can be clearly seen, that is, severe charge accumulation is generated in the sample to be measured under electron beam irradiation.
Therefore, when such a non-conductive material is subjected to scanning electron microscopy for high-power morphology observation, the most adopted means, in addition to the method of depositing a conductive film, is to select a balance voltage (V) corresponding to the material1And V2) Direct observation is performed, in which case the number of incident electrons is equal to the sum of the generated secondary electrons and the backscattered electrons, so that the surface of the sample is charge balanced, eliminating the charging phenomenon.
At present, the main method adopted at home and abroad is to continuously adjust the incident voltage of a scanning electron microscope and determine V according to experience2The value is obtained. When the acceleration voltage is greater than V2Secondary electrons and back scattering generated on the surface of the sampleThe total sum of the emitted electrons is less than the number of the incident electrons, and the surface is in a negative potential, so that more secondary electrons are received by the detector, and the image is bright; when the acceleration voltage is at V1And V2In between, the sum of the secondary electrons and the back scattered electrons generated on the surface of the sample is more than the number of the incident electrons, and the surface has a positive potential, so that the number of the secondary electrons received by the detector is reduced, and the image is blackened. However, the subjectivity of qualitative adjustment according to the brightness of the image is high, and the scanning electron microscope parameters need to be repeatedly and continuously adjusted by an operator, so that the efficiency is low.
Disclosure of Invention
The problems to be solved by the invention are as follows:
in view of the above problems, the present invention provides a method for calculating the uncharged equilibrium voltages V1 and V2 of the non-conductive ceramic material.
Means for solving the problems:
in order to solve the technical problem, the method for calculating the non-conductive ceramic material non-charge balance voltage comprises the following steps:
placing a sample to be detected of the non-conductor ceramic material on a sample stage of a scanning electron microscope, and setting the optimal working distance of X-ray energy spectrum analysis;
the incident acceleration voltage of the scanning electron microscope is continuously changed within the range from the lowest value to 5KV at specified intervals, and X-ray energy spectrum signals are respectively collected under different incident acceleration voltages;
storing all counting points of the acquired X-ray energy spectrum signals into a TXT format, introducing the counting points into a Matlab program, and calculating the upper limit voltage of the energy spectrum line corresponding to each X-ray energy spectrum signal by adopting linear fitting according to the upper limit Duane-Hunt principle of X-ray energy, namely performing linear fitting on the counting points at the tail end of the energy spectrum line;
and introducing the calculated upper limit voltage into a Matlab program for piecewise linear fitting, and calculating two intersection values of a piecewise fitting curve and a theoretical straight line, wherein the two intersection values are the uncharged equilibrium voltage of the sample to be detected.
According to the invention, the scanning electron microscope is adopted to combine with the X-ray energy spectrometerIn the form of a continuously regulated incident acceleration voltage at a lower acceleration voltage below 5 KV. And linearly fitting the counting points of the X-ray tail end spectral lines by adopting a Matlab program, and quantitatively calculating the upper limit voltage of the X-ray energy under different incident accelerating voltages. According to the principle of the upper limit of X-ray energy, namely the upper limit of X-ray spectral line energy theory is strictly equal to the real landing voltage value, linear piecewise fitting can be carried out on different upper limit voltages, and the uncharged equilibrium voltage V serving as the line segment intersection value can be quickly and quantitatively obtained1And V2And carrying out scanning electron microscope morphology observation and component analysis on the sample to be detected based on the two intersection points. Using the balance voltage V1And V2When a high-resolution morphology image of the non-conductor ceramic is shot, no charge phenomenon exists. Therefore, the method provided by the invention can be directly applied to the observation of the appearance of the scanning electron microscope of common ceramic samples and other non-conductive materials, and has the advantages of simple operation, accurate result and strong repeatability; further providing a scientific experimental method for deeply researching the microstructure of the nano material.
In the present invention, the specimen may be a polished surface or a polished cross section of the non-conductive ceramic material. Therefore, the surface to be detected of the sample to be detected can be ensured to be flat, pollution-free and scratch-free.
In the present invention, the magnification of the scanning electron microscope may be less than 1000 ×. Thus, the influence of sample drift can be reduced.
In the present invention, the minimum value of the incident acceleration voltage may be 350V, and the predetermined interval may be 100V or less. Thus, the uncharged equilibrium voltage can be more accurately fitted by increasing the total data volume.
In the present invention, the current value of the incident electron beam may be adjusted and fixed to 0.2nA, all the counts of the acquired X-ray spectrum signals may be higher than 500e ", and the acquisition time may be not longer than 500 s. Therefore, the influence of sample shift caused by charge in the long-time acquisition process of the X-ray energy spectrum can be reduced.
In the present invention, at least 100 or more count points of the upper limit voltage at the end of the spectral line may be selected and introduced into Matlab program for linear fitting. Therefore, the discrete degree of the counting points can be accurately analyzed, and the correlation coefficient of the fitting curve is improved.
In the present invention, the counting points may converge in an obvious linear manner, and the fitted correlation coefficient after fitting is greater than 0.95; if the fitting correlation coefficient is less than 0.95, the current of the incident electron beam is increased or the acquisition time is prolonged. Thereby, the convergence of the tail count point can be improved by increasing the total count point.
In the present invention, the piecewise linear fitting may be performed on the upper limit voltage with 1KV as a division point, and when the division point is selected, both of the two pieces of linear fitting correlation coefficients should be ensured to be greater than 0.95. This improves the accuracy of the equilibrium voltage calculated based on the piecewise fitting curve.
The invention has the following effects:
compared with the traditional image brightness and darkness adjusting method and the non-conductor ceramic material surface coating method, the method has the characteristics of simple operation, high accuracy and strong repeatability. Can directly and quantitatively calculate the optimal non-charge balance voltage V of the non-conductor ceramic materials1And V2. The balance voltage can be used for directly carrying out scanning electron microscope high-resolution morphology analysis and component analysis on the non-conductor ceramic sample. The foregoing and other objects, features, and advantages of the invention will be better understood from the following detailed description taken in conjunction with the accompanying drawings.
Drawings
FIG. 1 shows a spectrum of an X-ray energy spectrum signal of a lutetium aluminum garnet laser ceramic (LuAG) at an unbalanced voltage of 5KV according to an embodiment of the present invention;
FIG. 2 shows a distribution plot and a linear fit curve of 100 count points at the tail end of the spectral line corresponding to the X-ray spectral signal shown in FIG. 1;
in FIG. 3, a graph (a) shows the upper limit voltage E at 350V to 5KV calculated according to one embodiment of the present inventionDHLA distribution map of; graph (b) shows the upper limit voltage E in graph (a)DHLLinear simulation under 350V to 1KVCombining curves; graph (c) shows the upper limit voltage E in graph (a)DHLIs a linear fitting curve under 1KV to 5 KV;
in fig. 4, graph (a) shows lutetium aluminum garnet laser ceramic (LuAG) at equilibrium voltage V1Uncharged morphology at (560V); graph (b) shows lutetium aluminum garnet laser ceramic (LuAG) at equilibrium voltage V2The uncharged morphology under (3.1 KV);
fig. 5 shows the charged morphology of lutetium aluminum garnet laser ceramic (LuAG) at 5KV unbalanced voltage.
Detailed Description
The present invention is further described below in conjunction with the following embodiments and the accompanying drawings, it being understood that the drawings and the following embodiments are illustrative of the invention only and are not limiting. The same or corresponding reference numerals denote the same components in the respective drawings, and redundant description is omitted.
In order to solve the technical problem, the method for calculating the non-conductive ceramic material non-charge balance voltage comprises the following steps: placing a sample to be detected of the non-conductor ceramic material on a sample stage of a scanning electron microscope, and setting the optimal working distance of X-ray energy spectrum analysis; accelerating voltage E of incident light by scanning electron microscope0Continuously changing at regular intervals in the range of minimum value to 5KV and respectively corresponding to different incident accelerating voltages E0Collecting X-ray energy spectrum signals; storing the counting points of the acquired X-ray energy spectrum signals into a TXT format, introducing the counting points into a Matlab program, and calculating the upper limit voltage E of the energy spectrum line corresponding to each X-ray energy spectrum signal by adopting linear fitting according to the distance of the upper limit Duane-Hunt of the X-ray energyDHL(ii) a The calculated upper limit voltage EDHLIntroducing the sample into a Matlab program for piecewise linear fitting, and calculating two intersection values of a piecewise fitting curve and a theoretical straight line, wherein the two intersection values are the uncharged equilibrium voltage V of the sample to be detected1And V2。
Firstly, preparing a sample to be detected of the non-conductive ceramic material with polished surface or polished cross section. Specifically, the non-conductive ceramic material in the present embodiment is a bulk body, but is not limited thereto. The surface or the cross section of the sample to be detected is inlaid and polished, so that the surface to be detected (the plane to be detected) of the sample to be detected is flat, pollution-free and scratch-free and is parallel to the bottom surface. In the present invention, the sample of the non-conductive ceramic is lutetium aluminum garnet laser ceramic (LuAG), but is not limited thereto.
Placing the polished sample to be detected under a scanning electron microscope, adjusting the working distance of the scanning electron microscope to the optimal working distance for energy spectrum analysis, and enabling the scanning electron microscope to make the incident acceleration voltage E0Continuously changing at regular intervals in the range of minimum value to 5KV and respectively corresponding to different incident accelerating voltages E0And acquiring an X-ray energy spectrum signal. In the present invention, the magnification of the sem is less than 1000 ×, so that the influence of sample drift can be reduced, but is not limited thereto. In the invention, the X-ray energy spectrum has a certain counting rate and different incident accelerating voltages E0The lower count rate is the same and the incident acceleration voltage E0Should be larger than 1000 electrons. Thus, the discreteness of the linear fit can be reduced. Further, in the present invention, the incident acceleration voltage E0The minimum value is 350V, the maximum value is 5KV, the continuously-changed specified interval is less than 100V, and the current of the incident electron beam is adjusted to ensure that the dead time of the X-ray energy spectrometer is greater than 40 percent, so that the acquisition precision of the X-ray energy spectrum is ensured.
Then, calculating different incident accelerating voltages E according to the principle of the upper X-ray energy limit Duane-Hunt0Upper limit voltage E of lower X-ray energyDHL. At this time, it is ensured that the number of electrons incident on the surface of the sample to be examined is the same, and it is preferable to avoid the fitting data being discretely set to 500 electrons. Adjusting and fixing the current value of the incident electron beam to ensure different incident accelerating voltages E0The acquisition time for the incidence of the next 500 electrons is not more than 500s, and the total count of the acquired X-ray energy spectrum signals is higher than 500e-, preferably 0.2-1.0 nA. Therefore, the influence of sample shift caused by charge in the long-time acquisition process of the X-ray energy spectrum can be reduced.
And combining an X-ray energy spectrometer and adopting a region analysis mode to acquire spectral lines of the sample to be detected. Varying the incident acceleration voltage E0The analysis position should then be moved at a lower magnification. The X-ray spectrometer analysis preferably hasSample offset correction function. In the secondary electron mode, a lower magnification, for example, 100 × is selected to move and determine the position of the energy spectrum analysis, and the magnification of the energy spectrum acquisition image of the scanning electron microscope is preferably 500 × but not limited thereto.
The results of the X-ray spectroscopy were imported into the Matlab program for analysis. And (4) cutting the tail end of the spectral line of the drawn energy spectrum. The linear fitting analysis is carried out according to the principle of the upper X-ray energy limit Duane-Hunt. The counting point intercepted at the tail end is larger than 100, and the counting point at the tail end is better linear without obvious dispersion. The upper limit of the count point intercept should at least ensure that the correlation coefficient is greater than 0.95 after linear fitting. And if the fitting correlation coefficient is below 0.95, increasing the electron beam current or prolonging the acquisition time.
Then, different incident accelerating voltages E0Upper limit voltage E of linear fitting underDHLIntroduced into Matlab program for analysis, and E is shown0—EDHLAnd (5) distribution diagram. In the invention, 1KV is taken as a division point, and E is paired0—EDHLAnd (4) carrying out piecewise linear fitting on the points, and ensuring that the correlation coefficients of the two linear fits are both greater than 0.95 when the segmentation points are selected. Respectively calculating two linear functions, i.e. fitting straight line and conductor theoretical straight line E0=EDHLThe two intersection points are the balance voltage V1And V2。
Compared with the traditional image brightness and darkness adjusting method and the non-conductor ceramic material surface coating method, the method has the characteristics of simple operation, high accuracy and strong repeatability. Can directly and quantitatively calculate the optimal non-charge balance voltage V of the non-conductor ceramic materials1And V2. The balance voltage can be used for directly carrying out scanning electron microscope high-resolution morphology analysis and component analysis on the non-conductor ceramic sample. The foregoing and other objects, features, and advantages of the invention will be better understood from the following detailed description taken in conjunction with the accompanying drawings.
The present invention will be described in further detail with reference to specific examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
(example 1)
The method comprises the following steps: and taking a surface sample from the non-conductor ceramic sample, and mechanically polishing to ensure that the surface to be detected is flat and parallel to the bottom surface. In this example, the ceramic sample was a hot-pressed sintered lutetium aluminum garnet laser ceramic (LuAG).
Step two: on the basis of the first step, a sample surface does not need to be evaporated with a conductive film, the sample surface is placed on a sample table of a scanning electron microscope, and the working distance of the scanning electron microscope is adjusted to be the optimal value for X-ray energy spectrum collection; setting an incident acceleration voltage E0Is 5 KV; the current of the incident electron beam was 0.2 nA; the dead time of the spectrometer is guaranteed to be more than 40%. Specifically, fig. 1 shows a spectrum of an X-ray energy spectrum signal of a lutetium aluminum garnet laser ceramic (LuAG) at an unbalanced voltage of 5KV according to an embodiment of the present invention.
Step three: on the basis of the second step, under a secondary electron image mode, selecting a magnification factor of 500X, inserting an X-ray energy spectrum detector, setting the energy spectrum acquisition time to be 250s, and ensuring different incident acceleration voltages E0The number of the collected electrons is 500e-, and energy spectrum collection is carried out. Exchanging incident acceleration voltage E0The range is 400V to 5KV, the interval is 100V, and after the voltage parameter is adjusted, the sample is moved in a small range at the 100 multiplied descending position.
Step four: and on the basis of the third step, setting an X-ray energy spectrum acquisition region, wherein foreign matters are not in the region and the area is more than 100 multiplied by 100 microns.
Step five: on the basis of the step four, different incident accelerating voltages E are applied0And introducing the acquired X-ray spectral lines into a Matlab program for analysis. Linear fitting analysis is carried out according to the X-ray energy upper limit Duane-Hunt principle, and the termination energy of the spectral line under different accelerating voltages, namely the upper limit voltage, is calculatedPressure EDHL；
Specifically, the following command (1) is entered in the Matlab command window:
Step six: and analyzing the data in the step five, wherein the 100 counting points at the tail end of the X-ray energy spectrum line are obviously linearly converged, and the linear fitting related data is more than 0.95. If the counting point at the tail end is divergent, the acquisition time of the X-ray energy spectrum needs to be prolonged or the electron beam needs to be increased. In particular, fig. 2 shows a distribution plot and a linear fit curve of 100 count points at the tail end of the spectral line to which the X-ray spectral signal corresponds.
Step seven: after the sixth step is satisfied, 46 groups of different incident accelerating voltages E in the range of 350V to 5KV are obtained0Upper limit Duane-Hunt value of X-ray energy, i.e. upper limit voltage EDHLStored as EXCEL data and imported into Matlab program for analysis.
Step eight: on the basis of step seven, 46 groups of upper limit voltages EDHLPerforming piecewise linear fitting by using 1KV as a dividing point, and calculating a fitting straight line and a theoretical straight line E0=EDHLThe crossing point of (A) is the equilibrium voltage V of the lutetium aluminum garnet laser ceramic (LuAG)1And V2(ii) a Specifically, in FIG. 3, the graph (a) shows the upper limit voltage E at 350V to 5KV calculated according to one embodiment of the present inventionDHLA distribution map of; graph (b) shows the upper limit voltage E in graph (a)DHLA linear fitting curve when the curve is 350V to below 1 KV; graph (c) shows the upper limit voltage E in graph (a)DHLIs a linear fitting curve under 1KV to 5 KV;
specifically, the following command (2) is entered in the Matlab command window:
In this embodiment, after calculation, the uncharged equilibrium voltage V1And V2560V and 3.1KV respectively. Specifically, in fig. 4, graph (a) shows lutetium aluminum garnet laser ceramic (LuAG) at equilibrium voltage V1Uncharged morphology at (560V); graph (b) shows lutetium aluminum garnet laser ceramic (LuAG) at equilibrium voltage V2Uncharged morphology under (3.1 KV).
Step nine: and analyzing the linear fitting result obtained in the step eight, wherein the correlation coefficient is more than 0.95, so that the precision of the fitting result is further ensured.
Step ten: on the basis of the ninth step, the calculated uncharged equilibrium voltage V is adopted1And V2The ceramic sample is observed in the shape of a scanning electron microscope, and a high-resolution shape image can be directly shot. Therefore, the method can be conveniently used for calculating the balance voltage value of common non-conductor ceramic materials, and provides reliable guarantee for the microstructure analysis of the ceramic materials. In particular to
According to the invention, the incident acceleration voltage E0 is continuously adjusted at a lower acceleration voltage lower than 5KV by adopting a form of combining a scanning electron microscope and an X-ray energy spectrometer. And linearly fitting the X-ray tail end spectral line by adopting a Matlab program, and quantitatively calculating the upper limit voltage of the X-ray energy under different incident acceleration voltages E0. According to the principle of the upper limit of X-ray energy, namely the upper limit of X-ray spectral line energy theory is strictly equal to the real landing voltage value, linear piecewise fitting can be carried out on different upper limit voltages, and the uncharged equilibrium voltage V serving as the line segment intersection value can be quickly and quantitatively obtained1And V2And carrying out scanning electron microscope morphology observation and component analysis on the sample to be detected based on the two intersections. Using the balance voltage V1And V2When a high-resolution morphology image of the non-conductor ceramic is shot, no charge phenomenon exists. Therefore, the method provided by the invention can be directly applied to the observation of the appearance of the scanning electron microscope of common ceramic samples and other non-conductive materials, and has the advantages of simple operation, accurate result and strong repeatability.
The above embodiments are intended to illustrate and not to limit the scope of the invention, which is defined by the claims, but rather by the claims, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.
Claims (8)
1. A method for calculating the non-charge balance voltage of a non-conductive ceramic material comprises the following steps:
placing a sample to be detected of the non-conductor ceramic material on a sample stage of a scanning electron microscope, and setting the optimal working distance of X-ray energy spectrum analysis;
the incident acceleration voltage of the scanning electron microscope is continuously changed within the range from the lowest value to 5KV at specified intervals, and X-ray energy spectrum signals are respectively collected under different incident acceleration voltages;
storing all counting points of the acquired X-ray energy spectrum signals into a TXT format, introducing the counting points into a Matlab program, and calculating the upper limit voltage of the energy spectrum line corresponding to each X-ray energy spectrum signal by adopting linear fitting according to the upper limit Duane-Hunt principle of X-ray energy, namely performing linear fitting on the counting points at the tail end of the energy spectrum line;
and introducing the calculated upper limit voltage into a Matlab program for piecewise linear fitting, and calculating two intersection values of a piecewise fitting curve and a theoretical straight line, wherein the two intersection values are the uncharged equilibrium voltage of the sample to be detected.
2. The method for calculating the uncharged equilibrium voltage of the non-conductive ceramic material according to claim 1,
the sample to be detected is the polished surface or cross section of the non-conductive ceramic material.
3. The method for calculating the uncharged equilibrium voltage of the non-conductive ceramic material according to claim 1,
the magnification of the scanning electron microscope is less than 1000 x.
4. The method for calculating the uncharged equilibrium voltage of the non-conductive ceramic material according to claim 1,
the minimum value of the incident acceleration voltage is 350V, and the predetermined interval is 100V or less.
5. The method for calculating the uncharged equilibrium voltage of the non-conductive ceramic material according to claim 1,
adjusting and fixing the current value of the incident electron beam to be 0.2nA, acquiring all the counts of the X-ray energy spectrum signals to be higher than 500e-, and acquiring time not more than 500 s.
6. The method for calculating the uncharged equilibrium voltage of the non-conductive ceramic material according to claim 1,
during operation, selecting counting points of more than 100 of the upper limit voltage at the tail end of the energy spectrum line, and introducing the counting points into a Matlab program for linear fitting.
7. The method for calculating the uncharged equilibrium voltage of the non-conductive ceramic material according to claim 1,
the counting points are obviously linearly converged, and the fitting correlation coefficient after fitting is more than 0.95; if the fitting correlation coefficient is less than 0.95, the current of the incident electron beam is increased or the acquisition time is prolonged.
8. The method for calculating the uncharged equilibrium voltage of the non-conductive ceramic material according to claim 1,
and carrying out piecewise linear fitting on the upper limit voltage by taking 1KV as a dividing point, and ensuring that the correlation coefficients of the two linear fittings are both greater than 0.95 when the dividing point is selected.
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