Element concentration testing method based on testing device, and electronic device

Abstract

The present invention relates to the technical field of ion mass spectrometry detection. Disclosed are an element concentration testing method based on a testing device, and an electronic device. The method comprises: acquiring the most abundant isotope of an element to be tested in a test sample; when there is an interference signal of the most abundant isotope in the current test signal obtained by using a testing device to test the test sample, acquiring a mass resolution required for filtering the interference signal of the most abundant isotope when measuring the most abundant isotope, and denoting same as a first mass resolution; when the first mass resolution satisfies a first preset condition, setting the first mass resolution as the current mass resolution of the testing device to obtain concentration information of said element; and when there is an interference signal of the most abundant isotope in the current test signal and the first mass resolution does not satisfy the first preset condition, on the basis of concentration information of other isotopes of said element, obtaining the concentration information of said element. Using the present solution can improve the accuracy of element concentration measurement.

Description

Element concentration testing method based on testing device and electronic device

[0001] This application claims priority to the Chinese patent application No. CN202411082141.2, filed on August 08, 2024, which is incorporated by reference in its entirety. TECHNICAL FIELD

[0002] The present application relates to the field of ion mass spectrometry, for example to an element concentration testing method based on a testing device and an electronic device. BACKGROUND

[0003] Secondary ion mass spectroscopy (SIMS) uses a focused high-energy ion beam to bombard the sample, the composition on the surface of the sample is sputtered and ionized to produce secondary ions, and different mass-to-charge ratio secondary ions are separated by electric field, magnetic field or time of flight, and then the ion signals of interest are selectively received. It is an effective technical means for detecting impurity element content in solid materials. The generated secondary ions include single-atom monovalent positive or negative ions, and multi-atom monovalent or multivalent positive or negative ions. In general, ion counters are used to receive single-atom monovalent secondary ions, but multi-atom ions with similar mass-to-charge ratios can cause signal interference, making the ion signal intensity of the target element too high, resulting in a large deviation in the element concentration correction result.

[0004] For materials with complex composition, especially alloy materials, the mass number of the contained elements is often large, so the required mass resolution for distinguishing ions and ion groups with similar mass-to-charge ratios is larger. The best mass resolution capability of the commonly used magnetic SIMS for solid material composition analysis and impurity element content detection only reaches ~20000 (10% signal height). The mass resolution capability of a magnetic mass spectrometer refers to the ability to distinguish ions or ion groups with similar mass-to-charge ratios, which is usually related to the magnetic field density and deflection radius. The definition of mass resolution capability is M / ΔM, where M is the mass number and ΔM is the mass difference (assuming one unit of charge) of ions or ion groups with similar mass-to-charge ratios. Moreover, the higher the mass resolution of SIMS during testing, the lower the ion transmission efficiency, and the lower the amount of secondary ion signals received by the ion detector, resulting in a decrease in the sensitivity of element detection. In addition, it should be noted that the higher the mass resolution, the higher the stability requirements for the equipment and laboratory environment. Therefore, the detection of impurity elements that are severely mass-interfered and difficult to distinguish by magnetic mass spectrometry is currently a barrier to SIMS testing technology. SUMMARY

[0005] The element concentration test method based on a test device and the electronic device can improve the accuracy of element concentration detection, optimize the analysis method when the to-be-tested element contains mass interference and high or ultrahigh mass resolution is required, reduce the higher requirement for the performance of the device, and realize element concentration testing.

[0006] The purpose of the present application is achieved by adopting the following technical solutions:

[0007] The element concentration test method based on a test device is provided, and the method comprises the following steps:

[0008] Obtaining the highest abundance isotope of the to-be-tested element in the test sample; wherein the highest abundance isotope is the isotope with the highest abundance among the isotopes of the to-be-tested element;

[0009] When the interference signal of the highest abundance isotope exists in the current test signal obtained by testing the test sample by using the test device, obtaining the mass resolution required for filtering the interference signal of the highest abundance isotope when measuring the highest abundance isotope, and denoted as a first mass resolution;

[0010] When the first mass resolution meets a first preset condition, setting the first mass resolution as the current mass resolution of the test device, so as to obtain the concentration information of the highest abundance isotope, and obtaining the concentration information of the to-be-tested element according to the concentration information of the highest abundance isotope;

[0011] When the interference signal of the highest abundance isotope exists in the current test signal and the first mass resolution does not meet the first preset condition, obtaining the concentration information of the to-be-tested element based on the concentration information of other isotopes of the to-be-tested element.

[0012] In some possible implementation manners, the obtaining of the concentration information of the to-be-tested element based on the concentration information of other isotopes of the to-be-tested element comprises:

[0013] When the to-be-tested element has at least two isotopes, selecting other isotopes except the highest abundance isotope as a current test isotope;

[0014] When the interference signal of the current test isotope exists in the current test signal, obtaining the mass resolution required for filtering the interference signal of the current test isotope when measuring the current test isotope, and denoted as a second mass resolution;

[0015] when the second mass resolution meets a second preset condition, setting the second mass resolution as a current mass resolution of the test device to obtain concentration information of a current test isotope, and obtaining concentration information of the element to be measured according to the concentration information of the current test isotope;

[0016] when the second mass resolution does not meet the second preset condition, obtaining the concentration information of the element to be measured based on signal strengths of isotopes of interfering elements in the interference signal.

[0017] In some possible implementation manners, the obtaining of the concentration information of the element to be measured based on the signal strengths of the isotopes of the interfering elements in the interference signal comprises:

[0018] respectively obtaining signal strength ratios of a plurality of isotopes of each of the interfering elements, and calculating content ratio values of the isotopes of the interfering elements according to the signal strength ratios;

[0019] generating the concentration information of the element to be measured according to the content ratio values of the isotopes of the interfering elements, the measured signal strength of the element to be measured, and the signal strength of the interference signal.

[0020] In some possible implementation manners, the generating of the concentration information of the element to be measured according to the content ratio values of the isotopes of the interfering elements, the measured signal strength of the element to be measured, and the signal strength of the interference signal comprises:

[0021] obtaining a true signal strength of the element to be measured based on the content ratio values of the isotopes of the interfering elements, the measured signal strength of the element to be measured, and the signal strength of the interference signal;

[0022] obtaining a true signal strength of the element to be measured in a standard sample, denoted as a standard true signal strength;

[0023] obtaining the concentration information of the element to be measured in the test sample based on the true signal strength of the element to be measured in the test sample and the standard true signal strength;

[0024] In some possible implementation manners, the obtaining of the true signal strength of the element to be measured based on the content ratio values of the isotopes of the interfering elements, the measured signal strength of the element to be measured, and the signal strength of the interference signal comprises:

[0025] calculating content ratio values of the isotopes of all the interfering elements to obtain an adjustment coefficient;

[0026] calculating a product of the adjustment coefficient and the signal strength of the interference signal to obtain an adjusted interference signal strength;

[0027] calculating an absolute difference between the adjusted interference signal intensity and the measured signal intensity of the element to be detected, to obtain a true signal intensity of the element to be detected.

[0028] In some possible implementation manners, the obtaining of the concentration information of the element to be detected in the test sample based on the true signal intensity of the element to be detected in the test sample and the standard true signal intensity includes:

[0029] calculating a relative sensitivity factor based on the standard true signal intensity;

[0030] calculating the concentration information of the element to be detected in the test sample based on the relative sensitivity factor and the true signal intensity of the element to be detected in the test sample.

[0031] In some possible implementation manners, the method further includes:

[0032] when the element to be detected has one isotope, obtaining the concentration information of the element to be detected based on a signal intensity of an isotope of an interference element in the interference signal; or,

[0033] when the element to be detected has at least three isotopes, the interference signal of the current test isotope exists in the current test signal, and an absolute difference between a maximum resolution of the test device and a required resolution of the mass of the current test isotope is less than or equal to a third preset threshold, obtaining the concentration information of the element to be detected based on a signal intensity of an isotope of an interference element in the interference signal.

[0034] In some possible implementation manners, before the obtaining of the concentration information of the element to be detected based on the signal intensity of the isotope of the interference element in the interference signal, the method further includes:

[0035] determining whether the element to be detected has other isotopes in the main interference signal;

[0036] if yes, determining whether the isotopic interference signal has a mass interference signal; or,

[0037] whether the third mass resolution meets a third preset condition;

[0038] if the isotopic interference signal does not have the mass interference signal or the third mass resolution meets the third preset condition, determining whether the element to be detected has other interference signals in addition to the main interference signal;

[0039] if the element to be detected has other interference signals in addition to the main interference signal, selecting a maximum value of a mass resolution required for eliminating the other interference signals and the third mass resolution as a current test resolution;

[0040] If there is no other interference signal except the main interference signal of the to-be-tested element, the third quality resolution is selected as the current test resolution, so that the test device tests the test sample using the current test resolution.

[0041] The main interference signal is a signal with the highest signal strength in the interference signal of the to-be-tested element; the co-interference signal is a signal corresponding to an ion / ion group composed of other isotopes of the interference element in the main interference signal; the third quality resolution is a quality resolution required for filtering the co-interference signal; and the third preset condition includes that the third quality resolution is less than the maximum quality resolution of the test device and the absolute difference between the third quality resolution and the maximum quality resolution is greater than a third preset value.

[0042] In some possible implementation manners, the method further includes:

[0043] When there is no interference signal of one or more isotopes of the to-be-tested element in the current test signal, concentration information of an isotope with the highest abundance among all isotopes without the interference signal is obtained, and the concentration information of the to-be-tested element is obtained according to the concentration information of the isotope with the highest abundance among all isotopes without the interference signal.

[0044] The first preset condition includes that the maximum resolution of the test device is greater than the first quality resolution, and the absolute difference between the maximum resolution of the test device and the first quality resolution is greater than a first preset threshold.

[0045] The second preset condition includes that the maximum resolution of the test device is greater than the second quality resolution, and the absolute difference between the maximum resolution of the test device and the second quality resolution is greater than a second preset threshold.

[0046] The present application provides an electronic device, which comprises a memory and a processor, the memory stores a computer program, and the processor implements the steps of any method of the present application when executing the computer program.

[0047] Compared with the prior art, the application has at least the following beneficial effects: the application optimizes the analysis method for SIMS in the case that the element to be tested contains mass interference and high or ultra-high mass resolution is required, reduces the higher requirement for the performance of the equipment, tests other isotopes of the element to be tested, obtains accurate signal values of the element to be tested under the condition of lower mass resolution, obtains more real signal values of the element to be tested by testing the signal values of ions or ion groups composed of other isotopes of the interfering ions or ion groups, calculating the real signal strength of the interfering ions or ion groups through the content relationship, and deducting the mass interference signal, realizes the target element SIMS test of the element to be tested which can be screened out only by the ultra-high mass resolution of the equipment performance, determines the signal ratio of the isotopes through the content ratio of the isotopes, and avoids the difference between the isotope composition in the material and the isotope abundance value on the earth, and has guiding significance for the test of all mass spectrometers. BRIEF DESCRIPTION OF DRAWINGS

[0048] The application will be further described below in combination with the accompanying drawings and specific embodiments.

[0049] Fig. 1 is a flowchart of an embodiment of the element concentration test method based on a test device provided by the application;

[0050] Fig. 2 is a flowchart of another embodiment of the element concentration test method based on a test device provided by the application;

[0051] Fig. 3 is a flowchart of step S3 in the method provided by the application;

[0052] Fig. 4 is a flowchart of step S32 in the method provided by the application;

[0053] Fig. 5 is a flowchart of step S321 in the method provided by the application;

[0054] Fig. 6 is a structural schematic diagram of an electronic device provided by the application. DETAILED DESCRIPTION

[0055] Example implementations will now be described more fully with reference to the accompanying drawings. Example implementations may, however, be implemented in many different forms and should not be construed as limited to the implementations set forth herein; rather, these implementations are provided so that this disclosure will be thorough and complete, and fully convey the inventive aspects to those skilled in the art.

[0056] For the convenience of understanding, the main constituent elements (>1 at.%) of the test sample are defined as A, B, C, D, … in the application, each element contains several isotopes, and different isotopes of element A are defined as A1, A2, A3, A4, …, different isotopes of element B are defined as B1, B2, B3, B4, …, and so on. aA (A represents the relative atomic mass number) is expressed; the possible interference signals include the ions of the primary ion beam, such as the large amount of O2 generated by O primary ion analysis + The ion; the element to be measured is denoted as EX, and different isotopes of EX are denoted as EX1, EX2, EX3, …, EXf.

[0057] Please refer to Figure 1, Figure 1 is an embodiment of the element concentration test method provided by the test device based on the flowchart, the method comprises:

[0058] S11: Obtain the highest abundance isotope of the element to be measured in the test sample, and the highest abundance isotope is the isotope with the highest abundance among the isotopes of the element to be measured.

[0059] According to the isotope composition information of the element, the isotope with the highest abundance of the element to be measured in the test sample (denoted as EX1) is selected; the test device can be a SIMS device or other mass spectrometer capable of measuring element concentration.

[0060] S12: When the interference signal of the highest abundance isotope exists in the current test signal obtained by testing the test sample by using the test device, obtain the mass resolution required for filtering the interference signal of the highest abundance isotope when measuring the highest abundance isotope, denoted as the first mass resolution.

[0061] When testing by using the test device, due to the presence of other elements or compounds in the test sample, ions with mass numbers close to the highest abundance isotope of the element to be measured may be generated, thereby generating interference signals; based on this, it is judged whether the interference signal exists in the test signal (denoted as the current test signal) obtained by testing the test sample by using the test device, that is, whether the highest abundance isotope is interfered; if the highest abundance isotope is interfered (for example, the signals from other isotopes or molecules are overlapped), the mass resolution required to distinguish these interference signals is denoted as the first mass resolution.

[0062] S13: When the first mass resolution satisfies the first preset condition, the first mass resolution is set as the current mass resolution of the test device to obtain the concentration information of the highest abundance isotope; and according to the concentration information of the highest abundance isotope, the concentration information of the element to be measured is obtained.

[0063] If the first quality resolution satisfies the first preset condition (for example, the resolution of the testing device is sufficient to eliminate the interference of the interference signal), the first quality resolution is set as the current quality resolution of the testing device; then, the testing sample is tested at the first quality resolution, at which the testing device can accurately measure the concentration of the highest abundance isotope of the element to be tested, so as to obtain the concentration information of the element to be tested. Specifically, as to how to obtain the concentration information of the element to be tested by using the concentration information of the isotope of the element to be tested, assuming that the isotope of the element to be tested is denoted as H, the concentration information of the element to be tested is the concentration information of the isotope H / the abundance value of the isotope H.

[0064] Further, the testing sample is ion sputtered by using the adjusted testing device, and the generated secondary ions are collected; the ions then enter the mass analyzer, and are separated according to the mass / charge ratio thereof; at the first resolution, the mass analyzer can distinguish the highest abundance isotope from the possible interference signal, and ensure the accuracy of the measurement result.

[0065] It can be understood that the quality resolution of the testing device can be manually adjusted, in which case the operator of the testing device can be reminded by display and / or voice to adjust the current quality resolution to the first quality resolution; or the quality resolution of the testing device can also be automatically adjusted, in which case the first quality resolution is sent to the testing device after being calculated, so as to realize the automatic adjustment of the quality resolution.

[0066] S14: When the interference signal of the highest abundance isotope exists in the current testing signal and the first quality resolution does not satisfy the first preset condition, the concentration information of the element to be tested is obtained based on the concentration information of other isotopes of the element to be tested.

[0067] If the first quality resolution does not satisfy the preset condition (for example, the first quality resolution cannot be satisfied due to the limitation of the testing device), the concentration information of the highest abundance isotope cannot be directly measured; in this case, the concentration information of other isotopes of the element to be tested can be measured, so as to determine the concentration information of the element to be tested; although the abundance of these isotopes is relatively low, they can still provide useful information about the concentration of the element to be tested; by comprehensively considering the concentration information of these isotopes, the concentration information of the element to be tested can be estimated.

[0068] The embodiment can ensure that the test equipment can accurately measure the concentration of the highest abundance isotope of the element to be measured when the first mass resolution meets the first preset condition, and further provide accurate concentration information of the element to be measured. When the first mass resolution does not meet the first preset condition, the concentration measurement can be automatically switched to using other isotopes of the element to be measured. The scheme can maintain effectiveness under different conditions, reduce the limitations of the equipment, and improve the application range of the test. By first attempting to use the highest abundance isotope for testing and using a lower resolution equipment setting when possible, the accuracy can be ensured while optimizing resource utilization and reducing unnecessary equipment adjustment or upgrade requirements. By comprehensively considering the concentration information of multiple isotopes of the element to be measured, even in the case where the concentration of the element to be measured cannot be accurately measured directly through the highest abundance isotope, the concentration information of other isotopes with lower signal amounts can be measured to obtain the concentration information of the element to be measured, thereby enhancing the reliability of the test and the applicability of the measurement equipment.

[0069] Please refer to FIG. 2, which is a schematic diagram of another embodiment of the element concentration test method based on the test equipment provided by the application. The method comprises:

[0070] S21: Obtain the highest abundance isotope of the element to be measured in the test sample.

[0071] The highest abundance isotope is the isotope with the highest abundance among the isotopes of the element to be measured.

[0072] S22: Determine whether there is an interference signal of the highest abundance isotope in the current test signal obtained by testing the test sample using the test equipment.

[0073] When there is no interference signal of the highest abundance isotope in the current test signal, the concentration information of the highest abundance isotope is measured and further calculated to obtain the concentration information of the element to be measured.

[0074] S23: When there is an interference signal of the highest abundance isotope in the current test signal, obtain the mass resolution required for filtering the interference signal of the highest abundance isotope when measuring the highest abundance isotope, denoted as the first mass resolution.

[0075] S24: Determine whether the first mass resolution meets the first preset condition.

[0076] The first preset condition includes that the maximum resolution of the test equipment is greater than the first mass resolution, and the absolute difference between the maximum resolution of the test equipment and the first mass resolution is greater than a first preset threshold, that is, the maximum resolution of the test equipment can filter out the interference signal of the highest abundance isotope.

[0077] S25: setting the first mass resolution as the current mass resolution of the testing device to obtain the concentration information of the highest abundance isotope when the first mass resolution meets the first preset condition, and obtaining the concentration information of the element to be tested according to the concentration information of the highest abundance isotope.

[0078] S26: obtaining the concentration information of the element to be tested based on the concentration information of other isotopes of the element to be tested when the highest abundance isotope exists in the current testing signal and the first mass resolution does not meet the first preset condition.

[0079] When the first mass resolution approaches or exceeds the limit performance of the testing device, the testing device cannot filter out the interference signal of the highest abundance isotope, and at this time, the concentration information of the element to be tested can be obtained based on the concentration information of other isotopes of the element to be tested. Specifically, the following scheme can be used:

[0080] S261: determining whether the element to be tested has other isotopes.

[0081] The other isotopes are isotopes other than the highest abundance isotope.

[0082] S262: selecting other isotopes other than the highest abundance isotope as the current testing isotope when the element to be tested has at least two isotopes.

[0083] For example, when the element to be tested EX in the test sample has multiple isotopes (such as EX1, EX2, …, EXf), the best test scheme needs to be selected according to the characteristics of the isotopes and the ability of the testing device: using the calculation software to determine whether the highest abundance isotope EX1 is interfered by ions (such as: a A) or ion groups (such as: a A b B or a A b BBS) with similar mass-to-charge ratios; if the highest abundance isotope EX1 is interfered by ions or ion groups with similar mass-to-charge ratios and a very high mass resolution is required to filter out the interference signal, other isotopes of the element to be tested EX can be selected for testing to determine whether there is an interference signal and the required mass resolution.

[0084] S263: determining whether there is an interference signal of the current testing isotope in the current testing signal.

[0085] S264: obtaining the mass resolution required to filter out the interference signal of the current testing isotope when measuring the current testing isotope, denoted as the second mass resolution, when there is an interference signal of the current testing isotope in the current testing signal.

[0086] S265: determining whether the second mass resolution satisfies a second preset condition.

[0087] The second preset condition comprises that the maximum resolution of the testing device is greater than the second mass resolution, and an absolute difference between the maximum resolution of the testing device and the second mass resolution is greater than a second preset threshold value; the second preset threshold value can be equal to the first preset threshold value or can not be equal to the first preset threshold value; and the second preset threshold value is not limited herein.

[0088] S266: when the second mass resolution satisfies the second preset condition, setting the second mass resolution as the current mass resolution of the testing device to obtain the concentration information of the current testing isotope, and obtaining the concentration information of the element to be tested according to the concentration information of the current testing isotope.

[0089] In order to ensure a high signal strength, an isotope with the second highest abundance (denoted as a second-abundance isotope) among isotopes of the element to be tested can be selected as the current testing isotope, and it is determined whether the second-abundance isotope has an interference signal; if the second-abundance isotope has an interference signal, a mass resolution (denoted as a second mass resolution) required for filtering out the interference signal is determined. If the second mass resolution satisfies a second preset condition, the testing device tests the test sample at the second mass resolution to obtain the concentration information of the current testing isotope. If the second mass resolution does not satisfy the second preset condition, the current testing isotope is updated, for example, an isotope with the third highest abundance is selected as the current testing isotope, and S263-S266 are executed again until all isotopes of the element to be tested are traversed, or an isotope without an interference signal is found, and the loop is ended.

[0090] For example, assuming that an isotope EX2 of the element to be tested has an interference, a mass resolution (denoted as a second mass resolution MR2) required for filtering out the interference signal of the testing isotope EX2 is calculated; a comparison is made between the maximum resolution of the testing device and the second mass resolution MR2; if the second mass resolution MR2 is within the performance range of the testing device, and an absolute difference between the maximum resolution of the testing device and the second mass resolution MR2 is greater than a preset threshold value, the mass resolution of the testing device is adjusted to the second mass resolution MR2 for testing, a test signal at the mass resolution is obtained, and the concentration information of the current testing isotope is obtained from the test signal.

[0091] In an embodiment, when the second mass resolution does not satisfy the second preset condition, the concentration information of the element to be tested is obtained based on a signal strength of an isotope of an interference element in the interference signal.

[0092] In another embodiment, when the element to be measured has one isotope, the concentration information of the element to be measured is obtained based on the signal strength of the isotope of the interfering element in the interference signal through step S3.

[0093] In another embodiment, when the element to be measured has at least three isotopes, the interference signal of the current test isotope exists in the current test signal, and the absolute difference between the maximum resolution of the test device and the required resolution of the mass of the current test isotope is less than or equal to a third preset threshold, the test is performed through step S3.

[0094] Specifically, as shown in FIG. 3, which is a flowchart of step S3 in the method provided by the present application, the concentration information of the element to be measured can be obtained by using the following scheme:

[0095] S31: The test device with the same test parameters is used to test the test sample, and the signal strength ratio of each isotope of the interfering element is obtained respectively; and the content ratio of the isotopes of the interfering element is calculated according to the signal strength ratio.

[0096] The test parameter is the instrument parameter of the test device.

[0097] S32: The concentration information of the element to be measured is generated according to the content ratio of the isotopes of the interfering element, the measured signal strength of the element to be measured, and the signal strength of the interference signal.

[0098] As shown in FIG. 4, which is a flowchart of step S32 in the method provided by the present application, the concentration information of the element to be measured can be obtained by using the following scheme:

[0099] S321: The true signal strength of the element to be measured is obtained based on the content ratio of the isotopes of the interfering element, the measured signal strength of the element to be measured, and the signal strength of the interference signal.

[0100] As shown in FIG. 5, which is a flowchart of step S321 in the method provided by the present application, the true signal strength of the element to be measured can be obtained by using the following scheme:

[0101] S3211: The content ratio of the isotopes of all interfering elements is calculated to obtain an adjustment coefficient.

[0102] S3212: The product of the adjustment coefficient and the signal strength of the interference signal is calculated to obtain an adjusted interference signal strength; and the absolute difference between the adjusted interference signal strength and the measured signal strength of the element to be measured is calculated to obtain the true signal strength of the element to be measured.

[0103] The signal strength of the highest abundance isotope of the element to be measured in the test sample is selected as the measured signal strength of the element to be measured in the test sample.

[0104] For example, the ion group of the interfering element in the test sample is a1 A b1 B, which contains element A and element B.

[0105] By the ratio of the signal intensity of the two isotopes of element A a1 A and a2 A, the content ratio X of the two isotopes of element A is determined, and the calculation formula is as follows:

[0106] X = (signal intensity of isotope a1 A) / (signal intensity of isotope a2 A) (1)

[0107] By the ratio of the signal intensity of the two isotopes of element B b1 B and b2 B, the content ratio Y of the two isotopes of element B is determined:

[0108] Y = (signal intensity of isotope b1 B) / (signal intensity of isotope b2 B) (2)

[0109] Wherein, a1 A is the isotope of element A with the highest abundance, i.e. the isotope of A contained in the main interfering signal, a2 A preferentially selects the isotope of element A with the second highest abundance; b1 B is the isotope of element B with the highest abundance, i.e. the isotope of B contained in the main interfering signal, b2 B preferentially selects the isotope of element B with the second highest abundance.

[0110] It is worth noting that when measuring the signal intensity of the test isotope, multiple measurements can be made, and it is determined whether the deviation value of the signal intensity in the multiple measurement results is greater than the set deviation value (for example: 10%), if yes, the parameters of the test equipment need to be re-corrected to ensure the stability and accuracy of the test.

[0111] Further, the mass resolution required for filtering the interfering signal a2 A b2 B can be obtained first, if the test equipment can meet the mass resolution, the content ratios X and Y of the isotopes are obtained by the above algorithm; if the test equipment cannot meet the mass resolution, the isotope with the third highest abundance is selected as the element in the interfering signal, and the determination is continued in this way, until all isotopes of the interfering element are traversed, or the isotope of the interfering element that meets the condition is found to perform signal subtraction.

[0112] Taking the example that the above interfering signal contains two elements, the specific signal subtraction algorithm is as follows:

[0113] wherein, I EX is the true signal intensity of the element EX to be measured; M EX is the measured signal value of the element EX to be measured; X and Y are respectively a1 A / a2 A and b1 B / b2 the content ratio of B; is the signal intensity of the interfering ion group.

[0114] It can be understood that if the interfering signal contains more than two elements, for example, if the interfering signal contains three elements, the content ratio of the isotopes of the third element C is Z; then the above formula (3) is modified as: c1 C and c2 C.

[0115] By analogy, the corresponding calculation formula can be set based on the types of interfering elements.

[0116] The interference of the interfering ion group on the element EX to be measured is proportional to its own signal intensity, and is proportional to the isotope content ratio; by multiplying the isotope content ratio, the part of the interfering ion group that contributes to the signal of the element EX to be measured can be estimated, and this part of the interfering signal can be deducted from the measured signal value M EX . By deducting the interfering signal, the influence of the interfering ion group on the signal of the element to be measured can be eliminated or reduced, thereby improving the accuracy of the measurement; moreover, the interfering signal from different elements can be identified and deducted, enhancing the anti-interference ability of the test and making the test more reliable.

[0117] It is worth noting that generally, if the interfering signal contains only one element, it can be directly filtered out; if it cannot be filtered out, only the content ratio of the isotope of the element in the interfering signal is calculated and the signal is deducted; if the interfering signal contains more than two elements, the content ratio of the isotope of all elements in the interfering signal is calculated and the signal is deducted.

[0118] S322: Obtain the true signal intensity of the element to be measured in the standard sample, denoted as the standard true signal intensity.

[0119] The signal intensity of the highest abundance isotope of the element to be measured in the standard sample is selected as the true signal intensity of the element to be measured in the standard sample.

[0120] S323: Based on the true signal intensity of the element to be measured in the test sample and the standard true signal intensity, obtain the concentration information of the element to be measured in the test sample.

[0121] S3231: After the real signal intensity of the test sample and the standard real signal intensity of the element to be tested are used, the relative sensitivity factor is calculated.

[0122] The calculation of the relative sensitivity factor can refer to GB / T 25186-2010 Surface Chemical Analysis Secondary Ion Mass Spectrometry Determination of Relative Sensitivity Factor by Ion Implantation Reference Material or patent CN109755148B. The present application specifically provides the following two methods:

[0123] (a) The relative sensitivity factor is calculated by using the standard sample of ion implantation, as shown below:

[0124] Wherein, RSF is the relative sensitivity factor; m is the element to be tested in the standard sample; M is the matrix element as the reference; is the ion implantation dose, the unit is atoms / cm 2 ; is the signal intensity of the element to be tested EX at a depth of i, the unit is counts / s; I BG is the background signal intensity of the element to be tested EX, which can be obtained by testing the blank sample; the unit is counts / s; is the signal intensity of the matrix element M at a depth of i, the unit is counts / s; d is the total depth of the sputtering pit, the unit is cm; t is the sputtering time, the unit is s.

[0125] (b) The relative sensitivity factor RSF is calculated according to the matrix-doped standard substance, as shown below:

[0126] Wherein, C EX is the atomic concentration of the element to be tested EX, the unit is atoms / cm 3 ; I EX is the signal intensity of the element to be tested EX, the unit is counts / s; I M is the signal intensity of the matrix element M, the unit is counts / s.

[0127] S3232: The concentration information of the element to be tested in the test sample is calculated by using the relative sensitivity factor and the real signal intensity of the element to be tested.

[0128] The concentration of the element to be tested EX is obtained by the following formula:

[0129] Wherein, is the concentration of the element to be tested EX in the test sample, the unit is atoms / cm 3 ; RSF is the relative sensitivity factor; I EXis the true signal intensity of the element EX to be measured; I M is the signal intensity of the matrix element M; M is the matrix element taken as the reference; m is the element to be measured in the standard sample.

[0130] It is worth noting that the value of n depends on the calculation method of RSF and the element doping method of the sample, as follows:

[0131] (1) When ion-implanted samples are used as standard samples, if the test sample is prepared by doping growth, n is the abundance value of the measured isotope of the element m to be measured; if the test sample is an ion-implanted sample, n = 1.

[0132] (2) When uniformly doped samples are used as standard samples, if the test sample is prepared by doping growth, n = 1; if the test sample is an ion-implanted sample, n is the reciprocal of the abundance value of the measured isotope of the element m to be measured.

[0133] In element analysis of mass spectrometers (such as SIMS), in order to accurately calculate the concentration of the element EX to be measured, the relative sensitivity factor (RSF) and the true signal intensity of the element to be measured are needed; the relative sensitivity factor is a correction factor used to convert the measured signal into a concentration value, which takes into account the response differences of different elements in the mass spectrometer. First, the true signal intensity of the element EX to be measured is obtained, the true signal intensity is obtained by subtracting the interference signal, ensuring the accuracy of the data; a matrix element M is selected as a reference; the matrix element M is an element that widely exists in the sample and has a stable signal, which is used to standardize the measurement process; the signal intensity of the matrix element M is measured; the relative sensitivity factor RSF is used to correct the relationship between the signal intensity and the concentration; RSF is a parameter related to the element type, mass spectrometer settings and sample conditions, which describes the response sensitivity of the mass spectrometer to different elements; the value of RSF is usually determined by experiment, and standard samples or samples with known concentrations can be used for calibration.

[0134] The above scheme comprehensively considers the relative sensitivity factor and signal intensity, and can accurately calculate the concentration of the element to be measured, and obtain accurate and reliable concentration data, providing strong support for material analysis and chemical measurement.

[0135] In an embodiment, the following steps are further included before step S3:

[0136] S41, judging whether the element in the main interference signal of the element to be measured has other isotopes, the main interference signal being the signal with the highest signal intensity in the interference signal of the element to be measured.

[0137] S42, if the element in the main interference signal has other isotopes, judging whether the isotope interference signal has a mass interference signal.

[0138] The isotopic interference signal is a signal corresponding to an ion / ion pair composed of other isotopes of the interference element in the main interference signal; if the isotopic interference signal does not exist, the mass interference signal is executed in S44.

[0139] In S43, if the isotopic interference signal exists, it is determined whether the third mass resolution meets a third preset condition.

[0140] The third mass resolution is a mass resolution required for filtering the mass interference signal of the isotopic interference signal, and the third preset condition includes that the third mass resolution is less than a maximum mass resolution of the testing device and an absolute difference between the third mass resolution and the maximum mass resolution is greater than a third preset value.

[0141] In S44, it is determined whether the to-be-tested element has other interference signals in addition to the main interference signal.

[0142] In S45, if the to-be-tested element has other interference signals in addition to the main interference signal, a maximum value of a mass resolution required for eliminating the other interference signals and the third mass resolution is selected as a current testing resolution.

[0143] In S46, if the to-be-tested element does not have other interference signals in addition to the main interference signal, the third mass resolution is selected as the current testing resolution, so that the testing device uses the current testing resolution to test the test sample.

[0144] Further, if the mass resolution required for eliminating the main interference signal is high (for example, more than 20000), that is, the device does not meet the requirement of the mass resolution, and the interference element has no other isotopes, the testing condition is not met, and the testing is ended. Or, if the device resolution does not meet the mass resolution required for eliminating the main interference signal, and the device resolution also does not meet the mass resolution (that is, the third mass resolution) required for eliminating the isotopic interference signal, the testing condition is not met, and the testing is ended; if the device resolution does not meet the mass resolution required for eliminating the main interference signal, but the device resolution meets the mass resolution (that is, the third mass resolution) required for eliminating the isotopic interference signal, the testing is performed through step S3.

[0145] For example, under extreme conditions, the to-be-tested element EX contains only one stable isotope or contains other isotopes, but there is signal interference, and a very high mass resolution MR1 (>20000) is required to eliminate the mass interference signal, so it is extremely difficult to detect using a small magnetic SIMS; for example, a Ni-Cr-Al alloy material, the content of Y (yttrium) impurity element has a certain influence on the physical and chemical properties of the alloy, the Y element contains only one stable isotope 89 Y, mass interference signal 62 Ni 27Al requires a mass resolution of at least 22017 to be eliminated.

[0146] Suppose the main mass interference signal of element EX is a1 A b1 B, which requires a mass resolution of more than 20000 to be eliminated, and the ion groups of other isotopic compositions of element A and element B a2 A b2 B has no other mass interference or the mass interference signal only requires a relatively low mass resolution MR3 that can be met by the device.

[0147] If the above conditions are met, the concentration of the element to be measured is measured by step S3; the parameters of the test device are adjusted to appropriate values, and the appropriate mass resolution is selected to detect the element to be measured EX. Specifically, the mass resolution required to filter other interference signals other than the main interference signal (if any) is determined, while considering the mass resolution required to filter ions or ion groups of other isotopic compositions of interfering elements in the interference signal (i.e. isotopic interference signal) (i.e. third mass resolution), the maximum of the two mass resolutions needs to be selected as the lowest mass resolution for actual testing to ensure that the interference signal can be effectively filtered; if the element to be measured has no other interference signals other than the main interference signal, the third mass resolution is directly selected as the lowest mass resolution for actual testing.

[0148] In an embodiment, when there is no interference signal of one or more isotopes of the element to be measured in the current test signal, the concentration information of the isotope with the highest abundance among all isotopes without interference signals is obtained, and the concentration information of the element to be measured is obtained according to the concentration information of the isotope with the highest abundance among all isotopes without interference signals; For example: if there is no interference signal of the isotope with the highest abundance in the current test signal, the concentration of the isotope with the highest abundance is selected to obtain the concentration of the element to be measured; if there is no interference signal of the isotope with the second highest abundance in the current test signal, the concentration of the isotope with the second highest abundance is selected to obtain the concentration of the element to be measured, and so on.

[0149] The scheme can accurately obtain the concentration information of the element to be measured in the presence of interference signals by selecting a suitable mass resolution; improve the accuracy and reliability of the SIMS technology in the element concentration test of complex test samples; the scheme considers the possible interference signals of different isotopes and designs multiple test paths; by comprehensively considering the mass resolution required to filter the interference signals and the capability of the test equipment, the most suitable mass resolution is selected for testing, which can fully utilize the performance of the test equipment and avoid unnecessary waste of resources; when the highest abundance isotope exists interference, other isotopes can be selected for testing, which increases the flexibility and adaptability of the test method; when the direct measurement method of the isotope of the element to be measured is not feasible, the isotope signal intensity of the interference element is used to indirectly calculate the concentration of the element to be measured; by calculating the content ratio of the isotopes of the interference element, the influence of the interference signal on the signal intensity of the element to be measured can be removed, the accuracy of the concentration test is improved, the concentration of the element to be measured can be obtained by algorithm calculation according to the multiple isotope signals of the element to be measured and the interference element, and the types of elements that can be accurately tested by the SIMS technology are expanded; accurate identification of interference signals can help optimize test conditions, such as adjusting the mass resolution or selecting a more suitable isotope for testing; by identifying the main interference signal and the same interference signal, the interference degree can be quantified more accurately, and the concentration of the element to be measured can be more accurately inferred; the relative sensitivity factor is calculated by using the standard sample, and the concentration is calculated by combining the real signal intensity of the element to be measured, which can ensure the reliability and consistency of the measurement results.

[0150] In summary, the method provides a flexible, accurate and reliable element concentration test method by systematically considering and processing the interference signals in the SIMS test, especially in the processing of complex test samples, by correctly identifying and processing the interference signals, the accuracy and reliability of the test can be significantly improved, and the test method has a wide application prospect especially for the test requirements close to or exceeding the mass resolution capability of the test equipment.

[0151] Referring to FIG. 6, FIG. 6 is a structural schematic diagram of an electronic device provided by the present application. The electronic device 50 comprises one or more memories 51, one or more processors 52, and a bus connecting different platform systems.

[0152] The memory 51 can comprise a readable medium in the form of a volatile memory, such as a random access memory (RAM) 511 and / or a cache memory 512, and can further comprise a read-only memory (ROM) 513.

[0153] The memory 51 also stores a computer program, which can be executed by the processor 52 to enable the processor 52 to implement the steps of any of the above methods.

[0154] The memory 51 can also include a utilities 514 having one or more programs modules 515, such as an operating system, one or more application programs, other program modules, and program data, and each or a combination thereof can include implementation of a network environment.

[0155] Accordingly, the processor 52 can execute the above computer program, and can execute the utilities 514.

[0156] The processor 52 can employ one or more application specific integrated circuits (ASICs), DSPs, programmable logic devices (PLDs), complex programmable logic devices (CPLDs), field programmable gate arrays (FPGAs), or other electronic elements.

[0157] The bus can be one or more of several types of bus structures including a memory bus or memory controller, a peripheral bus, a graphics acceleration bus, a processor or local bus using any of a variety of bus architectures, and the like.

[0158] The electronic device 50 can also communicate with one or more external devices such as a keyboard or pointing device, a Bluetooth device, etc., one or more devices that enable

[0159] The embodiment of the present application further provides a computer readable storage medium for storing a computer program, the computer program being executed to implement the steps of the method in the embodiment of the present application, and the specific implementation manners and the achieved technical effects are the same as those of the method embodiment, and part of the content will not be described herein again.

[0160] In the present application, the readable storage medium can be any tangible medium containing or storing a program, which can be used or combined with an instruction execution system, device or apparatus. The program product can adopt any combination of one or more readable media. The readable medium can be a readable signal medium or a readable storage medium. The readable storage medium may, for example, be but is not limited to an electrical, magnetic, optical, electromagnetic, infrared, or semiconductor system, device or apparatus, or any combination of the above. More specific examples (non-exhaustive list) of the readable storage medium include an electrical connection having one or more wires, a portable disk, a hard disk, a random access memory (RAM), a read-only memory (ROM), an erasable programmable read-only memory (EPROM or flash memory), an optical fiber, a portable compact disk read-only memory (CD-ROM), an optical storage device, a magnetic storage device, or any suitable combination of the above.

[0161] The computer readable storage medium can include a data signal carried in the baseband or as a part of a carrier wave carrying the readable program code. Such a propagated data signal can take any of a variety of forms, including but not limited to electro-magnetic, optical, or any suitable combination thereof. The readable storage medium can also be any readable medium that can send, propagate or transfer the program for use by or in connection with an instruction execution system, apparatus or device. The program code contained on the readable storage medium can be transmitted using any suitable medium, including but not limited to wireless, wired, optical fiber, RF, or any suitable combination thereof. The program code for performing the operations of the present application can be written in any combination of one or more programming languages, including an object oriented programming language such as Java, C++, or the like, and conventional procedural programming languages, such as the C programming language or similar programming languages. The program code can execute entirely on the user's computing device, partly on the user's computing device, as a stand-alone software package, partly on the user's computing device and partly on a remote computing device or entirely on the remote computing device or server. In the case of the latter, the remote computing device can be connected to the user's computing device through any kind of network, including a local area network (LAN) or a wide area network (WAN), or the like, or can be connected to an external computing device (for example, using an Internet service provider to connect through the Internet).

Claims

1. A test device-based element concentration test method, the method comprising: obtaining a highest abundance isotope of a test element in a test sample; wherein the highest abundance isotope is an isotope of the test element with the highest abundance among isotopes of the test element; when an interference signal of the highest abundance isotope exists in a current test signal obtained by testing the test sample using the test device, obtaining a mass resolution required for filtering the interference signal of the highest abundance isotope when measuring the highest abundance isotope, denoted as a first mass resolution; when the first mass resolution satisfies a first preset condition, setting the first mass resolution as a current mass resolution of the test device to obtain concentration information of the highest abundance isotope; and obtaining concentration information of the test element according to the concentration information of the highest abundance isotope; when the interference signal of the highest abundance isotope exists in the current test signal and the first mass resolution does not satisfy the first preset condition, obtaining the concentration information of the test element based on concentration information of other isotopes of the test element.

2. The method of claim 1, wherein, The obtaining of the concentration information of the test element based on the concentration information of other isotopes of the test element comprises: when the test element has at least two isotopes, selecting an isotope other than the highest abundance isotope as a current test isotope; when an interference signal of the current test isotope exists in the current test signal, obtaining a mass resolution required for filtering the interference signal of the current test isotope when measuring the current test isotope, denoted as a second mass resolution; when the second mass resolution satisfies a second preset condition, setting the second mass resolution as the current mass resolution of the test device to obtain concentration information of the current test isotope, and obtaining the concentration information of the test element according to the concentration information of the current test isotope; when the second mass resolution does not satisfy the second preset condition, obtaining the concentration information of the test element based on signal strengths of isotopes of interference elements in the interference signal.

3. The method of claim 2, wherein, The obtaining of the concentration information of the test element based on the signal strengths of isotopes of interference elements in the interference signal comprises: obtaining signal strength ratios of a plurality of isotopes of each of the interference elements respectively, and calculating content ratio values of the isotopes of the interference elements according to the signal strength ratios; generating the concentration information of the test element according to the content ratio values of the isotopes of the interference elements, a measured signal strength of the test element, and a signal strength of the interference signal.

4. The method of claim 3, wherein, The generating of the concentration information of the test element according to the content ratio values of the isotopes of the interference elements, the measured signal strength of the test element, and the signal strength of the interference signal comprises: obtaining a true signal strength of the test element based on the content ratio values of the isotopes of the interference elements, the measured signal strength of the test element, and the signal strength of the interference signal; obtaining a true signal strength of the test element in a standard sample, denoted as a standard true signal strength; Based on the true signal intensity of the to-be-tested element in the test sample and the standard true signal intensity, concentration information of the to-be-tested element in the test sample is obtained.

5. The method of claim 4, wherein, The true signal intensity of the to-be-tested element is obtained based on the content ratio of the isotopes of the interference elements, the measured signal intensity of the to-be-tested element, and the signal intensity of the interference signal, and includes: The content ratio of the isotopes of all the interference elements is calculated to obtain an adjustment coefficient; The product of the adjustment coefficient and the signal intensity of the interference signal is calculated to obtain an adjusted interference signal intensity; The absolute difference between the adjusted interference signal intensity and the measured signal intensity of the to-be-tested element is calculated to obtain the true signal intensity of the to-be-tested element.

6. The method of claim 4, wherein, The concentration information of the to-be-tested element in the test sample is obtained based on the true signal intensity of the to-be-tested element in the test sample and the standard true signal intensity, and includes: Based on the standard true signal intensity, a relative sensitivity factor is calculated; Based on the relative sensitivity factor and the true signal intensity of the to-be-tested element in the test sample, the concentration information of the to-be-tested element in the test sample is calculated.

7. The method of claim 1, wherein, The method further includes: When the to-be-tested element has one isotope, the concentration information of the to-be-tested element is obtained based on the signal intensity of the isotope of the interference element in the interference signal; or, When the to-be-tested element has at least three isotopes, the current test signal has interference signal of the current test isotope, and the absolute difference between the maximum resolution of the test device and the required resolution of the mass of the current test isotope is less than or equal to a third preset threshold, the concentration information of the to-be-tested element is obtained based on the signal intensity of the isotope of the interference element in the interference signal.

8. The method of claim 1 or 7, wherein, Before the concentration information of the to-be-tested element is obtained based on the signal intensity of the isotope of the interference element in the interference signal, the method further includes: determining whether the to-be-tested element in the main interference signal has other isotopes; if yes, determining whether the isotope interference signal has mass interference signal; or, whether the third mass resolution meets the third preset condition; if the isotope interference signal does not have mass interference signal or the third mass resolution meets the third preset condition, determining whether the to-be-tested element has other interference signals in addition to the main interference signal; if the to-be-tested element has other interference signals in addition to the main interference signal, selecting the maximum value between the mass resolution required to eliminate the other interference signals and the third mass resolution as the current test resolution; if the to-be-tested element does not have other interference signals in addition to the main interference signal, selecting the third mass resolution as the current test resolution, so that the test device uses the current test resolution to test the test sample; The main interference signal is a signal with the highest signal strength in the interference signal of the to-be-tested element; the co-interference signal is a signal corresponding to an ion or ion group composed of other isotopes of the interference element in the main interference signal; the third mass resolution is a mass resolution required for filtering the mass interference signal of the co-interference signal, and the third preset condition includes that the third mass resolution is less than the maximum mass resolution of the testing device and an absolute difference between the third mass resolution and the maximum mass resolution is greater than a third preset value.

9. The method of claim 2, wherein, The method further includes: when the interference signal of one or more isotopes of the to-be-tested element does not exist in the current test signal, obtaining concentration information of an isotope with the highest abundance among all isotopes without the interference signal, and obtaining the concentration information of the to-be-tested element according to the concentration information of the isotope with the highest abundance among all isotopes without the interference signal; The first preset condition includes that the maximum resolution of the testing device is greater than the first mass resolution, and an absolute difference between the maximum resolution of the testing device and the first mass resolution is greater than a first preset threshold value. The second preset condition includes that the maximum resolution of the testing device is greater than the second mass resolution, and an absolute difference between the maximum resolution of the testing device and the second mass resolution is greater than a second preset threshold value. 10.An electronic device, comprising a memory and a processor, wherein the memory stores a computer program, and the processor implements the element concentration testing method based on a testing device according to any one of claims 1-9 when executing the computer program.

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