Parameter Error Calibration Method for Electron Probe Microanalysis Instrument

By using atomic lithography technology to prepare grating standard samples and directly calibrate the key parameters of the electron probe microanalysis instrument, the problem of large error accumulation in the existing technology is solved, and higher calibration accuracy and consistency are achieved, which is suitable for the precise measurement of three-dimensional nanostructures.

CN115877037BActive Publication Date: 2025-09-12SHANGHAI METROLOGY & TESTING TECHNOLOGY RESEARCH INSTITUTE CO LTD +1
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Patent Information

Application Number
CN202211365264.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-11-03
Publication Date
2025-09-12
Estimated Expiration
2042-11-03

AI Technical Summary

Technical Problem

Existing calibration methods for electron probe microanalysis instruments have the problem of difficulty in improving accuracy, especially in three-dimensional nanostructure measurements, where errors accumulate significantly, affecting device performance characterization.

Method used

A one-dimensional grating standard sample is prepared based on atomic lithography technology. By calculating the theoretical period value of the grating, the key parameters of the electron probe microanalysis instrument are directly calibrated, including the length measurement indication error and the sample stage repeatability error.

Benefits of technology

It shortens the length of the calibration traceability chain, reduces the error accumulation in the value transfer process, improves the calibration consistency and fusion measurement accuracy between different instruments, is easy to operate, and is suitable for precise measurement at the nanoscale.

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Abstract

The present invention discloses a parameter error calibration method for an electron probe microanalysis instrument. A one-dimensional grating standard template is prepared based on atomic lithography technology, and the theoretical grating period D of the one-dimensional grating standard template is calculated. The one-dimensional grating standard template is placed on the stage of the electron probe microanalysis instrument for a set time to maintain a stable test state. After the electron probe microanalysis instrument is clearly focused, the electron probe microanalysis instrument scans the one-dimensional grating standard template on the stage, captures and measures the grid spacing of the one-dimensional grating standard template, obtains a grating scanning distance measurement value L, and records the magnification at this time. Based on D and L, a calibration factor K at this magnification is calculated. The parameter error calibration method for an electron probe microanalysis instrument of the present invention shortens the traceability chain length for calibrating the instrument, reduces error accumulation in the measurement value transfer process, improves calibration consistency between different instruments, and is easy to operate.
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Description

Technical Field

[0001] The present invention relates to nanometer measurement technology, in particular to a parameter error calibration method of an electron probe microanalysis instrument. Background Art

[0002] Nanomanufacturing starts with measurement. As logic gate sizes in the semiconductor industry gradually approach the sub-10nm level, increasingly complex three-dimensional nanostructures are being manufactured. To ensure effective device performance, precise nanometrology techniques are required to accurately characterize and measure these micro- and nanostructures. In addition to non-imaging techniques such as X-rays and optical scattering, numerous microscopic techniques, such as scanning electron microscopy (SEM), electron probe analyzers, transmission electron microscopy (TEM), and atomic force microscopy (AFM), are also being applied to nanometrology.

[0003] Scanning electron microscopes and electron probe analyzers are both electron probe analysis instruments. They use a finely focused electron beam to scan across a sample. The resulting signals, such as secondary electrons, backscattered electrons, and X-rays at characteristic wavelengths of each element, are used to generate microscopic surface topography or to determine the concentration of the excited elements in the sample. For example, as device structures become increasingly three-dimensional, stereophotogrammetry is being used to extend SEM technology to three-dimensional (3D) nanometer measurements. When measuring nanostructures at different sample tilt angles relative to the beam, the lateral displacement of the nanostructures, as assessed from stereoscopic SEM image sets, can be used to calculate the height and 3D shape of the nanostructures. In this case, the SEM's measurement error in the lateral position of the nanostructures can significantly impact the measurement uncertainty of the 3D shape (especially when the solid angle is small). Furthermore, future approaches to measuring 3D nanostructures will require fused measurements, as no single instrument possesses all the capabilities (e.g., resolution, speed, and low uncertainty levels) required to characterize the full suite of parameters of complex nanostructures. Accurately matching different measurement instruments in fused measurements is a challenging issue, as data from these instruments must be shared in a complementary or collaborative manner to enhance metrological capabilities. Therefore, traceability calibration and accuracy improvement of different measuring instruments become crucial.

[0004] However, the existing length accuracy level of standard materials and the nanometer length value transfer method they define are important reasons that limit the calibration accuracy and consistency of electron probe analysis instruments. Taking China's current scanning electron microscope calibration specification (JJF1916-2021) as an example, the typical uncertainty of the 500nm standard sample used is 1.4nm. Similarly, the typical uncertainty of the 10μm standard sample period used by the electron probe microanalyzer is around 10nm. Due to the poor accuracy, uniformity and consistency of the above-mentioned standard samples themselves, on the one hand, they themselves bring about a large length error. On the other hand, since the grating needs to be calibrated by a measuring instrument containing a laser interferometer, there are many value transfer links and the error accumulation is also large. The above two reasons have made it difficult to improve the existing calibration accuracy of electron probe microanalyzers, which is a huge obstacle for the future three-dimensional characterization of sub-10nm device structures.

[0005] Directly traceable calibration methods and measurement transfer pathways based on natural constants offer solutions for improving calibration accuracy. In 2019, the silicon lattice constant was approved as a supplementary implementation of the "meter" at the nanoscale, enabling direct calibration of instruments such as TEMs, thereby improving measurement accuracy. However, conventional electron probe microanalysis instruments cannot achieve atomic resolution, making it impossible to directly use silicon lattice constants for direct traceable calibration. Therefore, exploring other novel, directly traceable calibration methods based on natural constants is crucial. Summary of the Invention

[0006] The technical problem to be solved by the present invention is to provide a parameter error calibration method for an electron probe microanalysis instrument, which shortens the traceability chain length for calibrating the instrument, reduces the error accumulation in the value transfer process, improves the calibration consistency between different instruments, is easy to operate, and helps to achieve flattening of value transfer. In addition, it is also of great significance for improving the accuracy of fusion measurement based on matching of different instruments.

[0007] To solve the above technical problems, the present invention provides a parameter error calibration method for an electron probe microanalysis instrument, which comprises the following steps:

[0008] S1. Prepare a one-dimensional grating standard sample based on atomic lithography technology and calculate the theoretical grating period D of the one-dimensional grating standard sample;

[0009] S2. The one-dimensional grating standard sample is placed on the stage of the electron probe microanalysis instrument to set the time so that the test state remains stable;

[0010] S3. After the electron probe microanalysis instrument is clearly focused, the electron probe microanalysis instrument scans the one-dimensional grating standard sample on the stage, captures and measures the grid spacing of the one-dimensional grating standard sample, obtains the grating scanning distance measurement value L, and records the magnification at this time;

[0011] S4. Calculate the calibration factor K of the electron probe microanalysis instrument at this magnification:

[0012]

[0013] Where: θ is the angle between the grating line direction and the scanning direction of the electron probe microanalysis instrument; N is the number of grating periods of the one-dimensional grating standard sample corresponding to the grating scanning distance measurement value L, and N is a positive integer;

[0014] S5. Using the calibration factor K, perform parameter calibration on the electron probe microanalysis instrument at the magnification.

[0015] Preferably, the parameters to be calibrated for the electron probe microanalysis instrument include length measurement indication error E1;

[0016] E1=|KL-L| / N.

[0017] Preferably, the parameters for calibration of the electron probe microanalysis instrument include the sample stage repeatability error E2;

[0018]

[0019] Where, is the average value of the center distance difference; Obtained through the following methods:

[0020] (1) Using the secondary electron image at the magnification, find a mark on the one-dimensional grating standard template, move the mark to the center of the screen, and capture the image after clear focus;

[0021] (2) Using the relative displacement method of the stage, move the stage in the X and Y directions by more than the set distance S, then move it back in the opposite directions by the same distance, and capture the image after it is clearly focused;

[0022] (3) measuring the distance between the current screen center position and the marked point;

[0023] (4) Repeat (1) to (3) M times, where M is a positive integer, and calculate the arithmetic mean of the M measurement results as the average value of the center distance difference

[0024] Preferably, M is 2, 3 or 4;

[0025] S>2D;

[0026] The magnification is 80k.

[0027] Preferably, in step S5, the linear distortion α is also calculated;

[0028]

[0029] Where ΔL max ΔL is the maximum value of the difference between the single period value at the center of the electron probe microanalysis instrument screen and the single period value at the four corners of the screen, max Obtained through the following methods:

[0030] (1) adjusting the magnification so that the length of a single grating period at the center of the one-dimensional grating standard sample is a set ratio of the maximum image amplitude, wherein the set ratio is 8% to 12%;

[0031] (2) Calculate the single grating period L0 of the one-dimensional grating standard sample at the center of the screen and the single grating periods L1, L2, L3, and L4 at the four corners of the screen;

[0032] (3)ΔL max =|ΔL i The maximum value in |, ΔL i =L i -L0, where i=1, 2, 3, 4.

[0033] Preferably, during the calibration process, the following conditions are preferred: ambient temperature: (20±5)°C, temperature fluctuation: ≤1°C / h, relative humidity: ≤75%.

[0034] Preferably, the electron probe microanalysis instrument is a scanning electron microscope, and the parameters to be calibrated include length measurement indication error.

[0035] Preferably, the electron probe microanalysis instrument is an electron probe analyzer, and the parameters to be calibrated include length measurement indication error and sample stage repeatability error.

[0036] Preferably, the set time is greater than 10 minutes.

[0037] Preferably, in step S1, a one-dimensional chromium grating standard sample is prepared based on chromium atom lithography technology, and the theoretical grating period value D of the standard sample is calculated using the chromium atom energy level transition frequency and the preparation process principle.

[0038] Preferably, the one-dimensional chromium grating standard sample is prepared based on chromium atom lithography technology, comprising the following steps:

[0039] S11. Heating the chromium powder to a temperature between 1550°C and 1650°C in a vacuum environment to sublime the powder and then extracting the powder from the discharge hole to form a Cr atom beam.

[0040] S12. The Cr atomic beam is collimated. The collimated Cr atomic beam 1 passes through a laser converging standing wave field orthogonal to the beam and is deposited onto the template under the action of a dipole force to form a one-dimensional chromium grating standard template 4.

[0041] Preferably, in step S12, the wavelength λ of laser 2 is 425.6 nm, and the resonance transition energy level of the Cr atom is The frequency of laser 2 is adjusted to the positive or negative detuning position of the center frequency corresponding to the resonance energy level; the theoretical grating period D of the formed one-dimensional chromium grating standard sample 4 is half of the wavelength λ of laser 2, which is 212.8nm.

[0042] Preferably, in step S3, N grid spacings are selected from the front of the image of the one-dimensional chrome grating standard template as the front grating scanning distance measurement value L1, and N grid spacings are selected from the rear of the image of the one-dimensional chrome grating standard template as the rear grating scanning distance measurement value L2;

[0043] The grating scanning distance measurement value L is the arithmetic average of the front grating scanning distance measurement value L1 and the rear grating scanning distance measurement value L2, that is, L = (L1 + L2) / 2.

[0044] Preferably, in step S2, the stage is rotated and kept horizontal;

[0045] The grating lines are in the front-to-back direction, and the electron probe microanalysis instrument is scanned in the left-right direction. The scanning direction of the electron probe microanalysis instrument is perpendicular to the direction of the grating lines, that is, θ=0°.

[0046] The parameter error calibration method of the electron probe microanalysis instrument of the present invention adopts a one-dimensional grating standard template prepared based on atomic lithography technology, and directly uses the theoretical period value of the grating to evaluate and calibrate the key parameters of the electron probe microanalysis instrument (the parameter evaluation and calibration process needs to refer to the relevant national metrology and calibration specifications), which can realize the direct evaluation and calibration of parameters such as the length measurement indication error, linear distortion, and sample stage repeatability error of the electron probe microanalysis instrument. The parameter error calibration method of the electron probe microanalysis instrument also has the advantage of in-situ calibration at any time (for example, in the process of characterizing the repeatability error of the sample stage, when measuring the distance between the current screen center position and the mark point, the grating theoretical period value D of the one-dimensional grating standard template can be directly used for determination, and the result will be more accurate and stable), and the advantage of direct traceability can be exerted many times in certain measurement processes (such as sample stage repeatability error measurement). This parameter error calibration method for electron probe microanalysis instruments shortens the traceability chain length for instrument calibration, reduces error accumulation in the measurement value transfer process, and improves calibration consistency between different instruments. It is easy to operate and helps to achieve flattening of measurement value transfer. It is also of great significance for improving the accuracy of fusion measurements based on matching different instruments. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] In order to more clearly illustrate the technical solution of the present invention, the following briefly introduces the drawings required for use in the present invention. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0048] Figure 1 Flowchart of an embodiment of a parameter error calibration method for an electron probe microanalysis instrument of the present invention;

[0049] Figure 2 A schematic diagram of a one-dimensional chromium grating standard sample photolithography process according to an embodiment of a parameter error calibration method for an electron probe microanalysis instrument of the present invention;

[0050] Figure 3 Schematic diagram of measurement calibration of an embodiment of a parameter error calibration method for an electron probe microanalysis instrument according to the present invention. DETAILED DESCRIPTION

[0051] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without creative work are within the scope of protection of the present invention.

[0052] The terms "first", "second" and similar words used in this application do not indicate any order, quantity or importance, but are only used to distinguish different components. Words such as "include" or "comprise" mean that the elements or objects preceding the word include the elements or objects listed after the word and their equivalents, without excluding other elements or objects. Words such as "connect" or "connected" are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "Up", "down", "left", "right" and the like are only used to indicate relative position relationships. When the absolute position of the object being described changes, the relative position relationship may also change accordingly.

[0053] It should be noted that, in the absence of conflict, the embodiments of the present invention and the features in the embodiments may be combined with each other.

[0054] Example 1

[0055] Parameter error calibration method of electron probe microanalysis instrument, such as Figure 1 As shown, it includes the following steps:

[0056] S1. Prepare a one-dimensional grating standard sample based on atomic lithography technology and calculate the theoretical grating period D of the one-dimensional grating standard sample;

[0057] S2. The one-dimensional grating standard sample is placed on the stage of the electron probe microanalysis instrument for a set time (eg, greater than 10 min, such as 20 min, 30 min, 43 min, etc.) to keep the test state stable;

[0058] S3. After the electron probe microanalysis instrument is clearly focused, the electron probe microanalysis instrument scans the one-dimensional grating standard sample on the stage, captures and measures the grid spacing of the one-dimensional grating standard sample, obtains the grating scanning distance measurement value L, and records the magnification at this time;

[0059] S4. Calculate the calibration factor K of the electron probe microanalysis instrument at this magnification:

[0060]

[0061] Where: θ is the angle between the grating line direction and the scanning direction of the electron probe microanalysis instrument; N is the number of grating periods of the one-dimensional grating standard sample corresponding to the grating scanning distance measurement value L, and N is a positive integer;

[0062] S5. Using the calibration factor K, perform parameter calibration on the electron probe microanalysis instrument at the magnification.

[0063] Preferably, the parameters to be calibrated for the electron probe microanalysis instrument include length measurement indication error E1;

[0064] E1=|KL-L| / N.

[0065] Preferably, the parameters for calibration of the electron probe microanalysis instrument include the sample stage repeatability error E2;

[0066]

[0067] Where, is the average value of the center distance difference; Obtained through the following methods:

[0068] (1) Using the secondary electron image at the magnification, find a mark on the one-dimensional grating standard template, move the mark to the center of the screen, and capture the image after clear focus;

[0069] (2) Using the relative displacement method of the stage, move the stage in the X and Y directions by more than the set distance S, then move it back in the opposite directions by the same distance, and capture the image after it is clearly focused;

[0070] (3) measuring the distance between the current screen center position and the marked point;

[0071] (4) Repeat (1) to (3) M times, where M is a positive integer, and calculate the arithmetic mean of the M measurement results as the average value of the center distance difference

[0072] Preferably, M is 2, 3 or 4;

[0073] S>2D;

[0074] The magnification is 80k.

[0075] Preferably, in step S5, the linear distortion α is also calculated;

[0076]

[0077] Where ΔL max ΔL is the maximum value of the difference between the single period value at the center of the electron probe microanalysis instrument screen and the single period value at the four corners of the screen, max Obtained through the following methods:

[0078] (1) adjusting the magnification so that the length of a single grating period at the center of the one-dimensional grating standard sample is a set ratio of the maximum image amplitude, wherein the set ratio is 8% to 12%;

[0079] (2) Calculate the single grating period L0 of the one-dimensional grating standard sample at the center of the screen and the single grating periods L1, L2, L3, and L4 at the four corners of the screen;

[0080] (3)ΔL max =|ΔL i The maximum value in |, ΔL i =L i -L0, where i=1, 2, 3, 4.

[0081] Preferably, the electron probe microanalysis instrument is a scanning electron microscope, and the parameters to be calibrated include length measurement indication error, etc.

[0082] Preferably, the electron probe microanalysis instrument is an electron probe analyzer, and the parameters to be calibrated include length measurement indication error and sample stage repeatability error.

[0083] The parameter error calibration method for this electron probe microanalysis instrument preferably maintains the following conditions during the calibration process: ambient temperature: (20±5)°C, temperature fluctuation: ≤1°C / h, and relative humidity: ≤75%. Furthermore, when selecting the image acquisition and measurement positions for the grid spacing of a one-dimensional grating standard sample, positions with holes, scratches, and contamination on the grating should be avoided as much as possible.

[0084] The parameter error calibration method of the electron probe microanalysis instrument of Example 1 is based on the atomic lithography technology to prepare a one-dimensional grating standard template and calculate its grating theoretical period value D; according to the grating scanning distance measurement value L and the grating theoretical period value D under the corresponding magnification, the calibration factor K of the electron probe microanalysis instrument at the magnification is calculated, and the electron probe microanalysis instrument is calibrated at the magnification using the calibration factor K. The grating structure prepared based on the atomic lithography technology has a strict correspondence between the atomic deposition position and the trough or antinode position of the laser standing wave field, so a one-dimensional grating structure with a highly accurate and reliable period can be prepared. The period of this structure is strictly traced back to the natural transition frequency between the transition energy levels of the atoms. The error is generally on the order of 0.1nm or less, and has very good intra-sample consistency and inter-sample consistency. Taking chromium atom lithography technology as an example, after verification by the National Institute of Standards and Technology of the United States, Tongji University, China National Institute of Metrology and other parties, its accuracy level is better than 0.1nm. It can be used directly without a fixed value within a certain range, and its scale is also compatible with electron probe microanalysis instruments. Therefore, this grating has the ability to develop a direct calibration method based on natural constants, which is of great significance for improving the accuracy level of electron probe microanalysis instruments.

[0085] The parameter error calibration method of the electron probe microanalysis instrument adopts a one-dimensional grating standard sample prepared based on atomic lithography technology, and directly uses the theoretical period value of the grating to evaluate and calibrate the key parameters of the electron probe microanalysis instrument (the parameter evaluation and calibration process must refer to the relevant national metrology and calibration specifications). It can realize the direct evaluation and calibration of parameters such as the length measurement indication error, linear distortion, and sample stage repeatability error of the electron probe microanalysis instrument. The parameter error calibration method of the electron probe microanalysis instrument also has the advantage of in-situ calibration at any time (for example, during the characterization of the sample stage repeatability error, when measuring the distance between the current screen center position and the marked point, the grating theoretical period value D of the one-dimensional grating standard sample can be directly used for setting the value, and the result will be more accurate and stable). In certain measurement processes (such as sample stage repeatability error measurement), the advantage of direct traceability can be exerted multiple times.

[0086] This parameter error calibration method for electron probe microanalysis instruments shortens the traceability chain length for instrument calibration, reduces error accumulation in the measurement value transfer process, and improves calibration consistency between different instruments. It is easy to operate and helps to achieve flattening of measurement value transfer. It is also of great significance for improving the accuracy of fusion measurements based on matching different instruments.

[0087] Example 2

[0088] Based on the parameter error calibration method of the electron probe microanalysis instrument in Example 1, in step S1, a one-dimensional chromium grating standard sample is prepared based on chromium atom lithography technology, and the grating theoretical period value D of the standard sample is calculated using the chromium atomic energy level transition frequency and the preparation process principle.

[0089] Better, such as Figure 2 As shown, the preparation of a one-dimensional chromium grating standard sample based on chromium atom lithography technology includes the following steps:

[0090] S11. Heating the chromium powder to a temperature between 1550°C and 1650°C in a vacuum environment to sublime the powder and then extracting the powder from the discharge hole to form a Cr atom beam.

[0091] S12. The Cr atomic beam is collimated by laser frequency locking and laser cooling. The collimated Cr atomic beam 1 passes through a laser converging standing wave field orthogonal to the beam and is deposited onto the template under the action of a dipole force to form a one-dimensional chromium grating standard template 4.

[0092] Preferably, in step S12, the wavelength λ of laser 2 is 425.6 nm, and the resonance transition energy level of the Cr atom is The frequency of laser 2 is adjusted to a positive detuning position (+20 MHz) or a negative detuning position (-250 MHz) corresponding to the center frequency of the resonance energy level. Therefore, the theoretical grating period D of the formed one-dimensional chromium grating standard sample 4 is half of the wavelength λ of laser 2, which is 212.8 nm.

[0093] The theoretical period value of the standard sample calculated using the chromium atomic energy level transition frequency and the preparation process principle is that the period of the self-traceable grating prepared by basic chromium atom lithography is 212.8nm, the period of the self-traceable grating prepared by polarization gradient type or positive and negative detuning type chromium atom lithography is 106.4nm, and the period of the self-traceable grating prepared by one-eighth wavelength chromium atom lithography is 53.2nm.

[0094] Example 3

[0095] Based on the parameter error calibration method of the electron probe microanalysis instrument of embodiment 1, Figure 3 As shown, in step S3, N grid spacings are selected from the front of the image of the one-dimensional chrome grating standard template as the front grating scanning distance measurement value L1, and N grid spacings are selected from the rear of the image of the one-dimensional chrome grating standard template as the rear grating scanning distance measurement value L2;

[0096] The raster scan distance measurement value L is the arithmetic average of the front raster scan distance measurement value L1 and the rear raster scan distance measurement value L2, that is, L = (L1 + L2) / 2. Multiple (eg, 5) measurements can be performed continuously to obtain the average value.

[0097] Preferably, in step S2, the stage is rotated and kept horizontal so that the electron beam is incident vertically on the grating;

[0098] The grating lines are in the front-to-back direction, and the electron probe microanalysis instrument is scanned in the left-right direction. The scanning direction of the electron probe microanalysis instrument is perpendicular to the direction of the grating lines, that is, θ=0°.

[0099] The stage can be rotated to perform angle correction so that the scanning direction of the electron probe microanalysis instrument is perpendicular to the direction of the grating lines, avoiding the angle error introduced by manually placing the one-dimensional grating standard sample. The actual length of the grating scanning distance measurement value L on the one-dimensional chromium grating standard sample should be ND, and the calibration factor K at this magnification is:

[0100]

[0101] In such Figure 3 At the 30K× magnification shown, the grating scanning distance measurement value L is 2081 nm, and the actual period value (D×N) of the entire measurement interval should be 212.8 nm×10=2128 nm. Therefore, the calibration factor K at this magnification is 1.022.

[0102] The complete calibration process needs to be performed in sequence at multiple different magnifications, and the calibration process is the same as above.

[0103] The above describes in detail the preferred embodiments of the present invention. It should be understood that those skilled in the art can make numerous modifications and variations based on the concepts of the present invention without inventive effort. Therefore, any technical solutions that can be derived by those skilled in the art through logical analysis, reasoning, or limited experimentation based on the concepts of the present invention and the prior art should be within the scope of protection defined by the claims.

Claims

1. A method for calibrating parameter errors of an electron probe microanalysis instrument, characterized in that: It includes the following steps: S1. Prepare a one-dimensional grating standard sample based on atomic lithography technology and calculate the theoretical grating period D of the one-dimensional grating standard sample; S2. The one-dimensional grating standard sample is placed on the stage of the electron probe microanalysis instrument to set the time so that the test state remains stable; S3. After the electron probe microanalysis instrument is clearly focused, the electron probe microanalysis instrument scans the one-dimensional grating standard sample on the stage, captures and measures the grid spacing of the one-dimensional grating standard sample, obtains the grating scanning distance measurement value L, and records the magnification at this time; S4. Calculate the calibration factor K of the electron probe microanalysis instrument at this magnification: Where: θ is the angle between the grating line direction and the scanning direction of the electron probe microanalysis instrument; N is the number of grating periods of the one-dimensional grating standard sample corresponding to the grating scanning distance measurement value L, and N is a positive integer; S5. Calibrate the parameters of the electron probe microanalysis instrument at the magnification using the calibration factor K; the calibration parameters of the electron probe microanalysis instrument include at least one of the length measurement indication error E1 and the sample stage repeatability error E2; E1=|KL-L| / N; Where, is the average of the center distance differences.

2. The parameter error calibration method of the electron probe microanalysis instrument according to claim 1, characterized in that: ΔS is obtained by the following method: (1) Using the secondary electron image at the magnification, find a mark on the one-dimensional grating standard template, move the mark to the center of the screen, and capture the image after clear focus; (2) Using the relative displacement method of the stage, move the stage in the X and Y directions by more than the set distance S, then move it back in the opposite directions by the same distance, and capture the image after it is clearly focused; (3) measuring the distance between the current screen center position and the marked point; (4) Repeat (1) to (3) M times, where M is a positive integer, and calculate the arithmetic mean of the M measurement results as the average value of the center distance difference 3. The parameter error calibration method of the electron probe microanalysis instrument according to claim 2, characterized in that: M is 2, 3 or 4; S>2D; The magnification is 80k.

4. The parameter error calibration method of the electron probe microanalysis instrument according to claim 1, characterized in that: In step S5, the linear distortion α is also calculated; Where ΔL max ΔL is the maximum value of the difference between the single period value at the center of the electron probe microanalysis instrument screen and the single period value at the four corners of the screen, max Obtained through the following methods: (1) adjusting the magnification so that the length of a single grating period at the center of the one-dimensional grating standard sample is a set ratio of the maximum image amplitude, wherein the set ratio is 8% to 12%; (2) Calculate the single grating period L0 of the one-dimensional grating standard sample at the center of the screen and the single grating periods L1, L2, L3, and L4 at the four corners of the screen; (3)ΔL max =|ΔL i The maximum value in |, ΔL i =L i -L0, where i=1, 2, 3, 4.

5. The parameter error calibration method of the electron probe microanalysis instrument according to claim 1, characterized in that: During the calibration process: ambient temperature: (20±5)℃, temperature fluctuation: ≤1℃ / h, relative humidity: ≤75%.

6. The parameter error calibration method of the electron probe microanalysis instrument according to claim 1, characterized in that: The electron probe microanalysis instrument is a scanning electron microscope, and the parameters to be calibrated include length measurement indication error.

7. The parameter error calibration method of the electron probe microanalysis instrument according to claim 1, characterized in that: The electron probe microanalysis instrument is an electron probe analyzer, and the parameters to be calibrated include length measurement indication error and sample stage repeatability error.

8. The parameter error calibration method of the electron probe microanalysis instrument according to claim 1, characterized in that: The set time is greater than 10 minutes.

9. The parameter error calibration method of the electron probe microanalysis instrument according to claim 1, characterized in that: In step S1, a one-dimensional chromium grating standard sample is prepared based on chromium atom lithography technology, and the theoretical grating period D of the standard sample is calculated using the chromium atomic energy level transition frequency and the preparation process principle.

10. The parameter error calibration method of the electron probe microanalysis instrument according to claim 9, characterized in that: The preparation of a one-dimensional chromium grating standard sample based on chromium atom lithography technology includes the following steps: S11. Heating the chromium powder to a temperature between 1550°C and 1650°C in a vacuum environment to sublime the powder and then extracting the powder from the discharge hole to form a Cr atom beam. S12. The Cr atomic beam is collimated. The collimated Cr atomic beam passes through a laser converging standing wave field orthogonal to the beam and is deposited onto a template under the action of a dipole force to form a one-dimensional chromium grating standard template.

11. The parameter error calibration method of the electron probe microanalysis instrument according to claim 10, characterized in that: In step S12, the laser wavelength λ is 425.6 nm, and the corresponding resonant transition energy level of the Cr atom is The laser frequency is adjusted to a positive detuning or negative detuning position corresponding to the center frequency of the resonant transition energy level; the grating theoretical period value D of the formed one-dimensional chromium grating standard sample is half of the laser wavelength λ, which is 212.8nm.

12. The parameter error calibration method of the electron probe microanalysis instrument according to claim 1, characterized in that: In step S3, N grid spacings are selected from the front of the image of the one-dimensional chrome grating standard template as the front grating scanning distance measurement value L1, and N grid spacings are selected from the rear of the image of the one-dimensional chrome grating standard template as the rear grating scanning distance measurement value L2; The grating scanning distance measurement value L is the arithmetic average of the front grating scanning distance measurement value L1 and the rear grating scanning distance measurement value L2, that is, L = (L1 + L2) / 2.

13. The parameter error calibration method of the electron probe microanalysis instrument according to claim 1, characterized in that: In step S2, the stage is rotated and kept horizontal; The grating lines are in the front-to-back direction, and the electron probe microanalysis instrument is scanned in the left-right direction. The scanning direction of the electron probe microanalysis instrument is perpendicular to the direction of the grating lines, that is, θ=0°.

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