A method for quantitatively analyzing fissile nuclide Zr based on SIMS

Abstract

The application belongs to the technical field of irradiation effect of nuclear fuel and material, and particularly relates to a fissile nuclide Zr quantitative analysis method based on SIMS. 90 Zr + Ion implantation, coating treatment of the surface of the CeO2 sample after ion implantation, optimization adjustment of SIMS analysis parameters, depth profiling and concentration calibration of fissile nuclide Zr in the CeO2 sample. 90 The method can quickly test and obtain the concentration distribution of fissile nuclide Zr in the depth direction of the CeO2 simulation fuel, the relative sensitivity factor and the detection limit. 90 The method can be used for the characterization analysis of fissile nuclide Zr in the irradiated nuclear fuel, and the obtained relative sensitivity factor of fissile nuclide Zr can be used for the concentration calibration of the secondary ion intensity of fissile nuclide Zr in the irradiated nuclear fuel at different radial positions along with the depth change curve, so as to obtain the concentration distribution of fissile nuclide Zr along the radial direction in the irradiated nuclear fuel. 90 The method can be used for the characterization analysis of fissile nuclide Zr in the irradiated nuclear fuel, and the obtained relative sensitivity factor of fissile nuclide Zr can be used for the concentration calibration of the secondary ion intensity of fissile nuclide Zr in the irradiated nuclear fuel at different radial positions along with the depth change curve, so as to obtain the concentration distribution of fissile nuclide Zr along the radial direction in the irradiated nuclear fuel. 90 The method can be used for the characterization analysis of fissile nuclide Zr in the irradiated nuclear fuel, and the obtained relative sensitivity factor of fissile nuclide Zr can be used for the concentration calibration of the secondary ion intensity of fissile nuclide Zr in the irradiated nuclear fuel at different radial positions along with the depth change curve, so as to obtain the concentration distribution of fissile nuclide Zr along the radial direction in the irradiated nuclear fuel.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of irradiation effects of nuclear fuels and materials, and particularly relates to a fissile nuclide Zr quantitative analysis method based on SIMS. BACKGROUND

[0002] During the irradiation process in the reactor, a large amount of zirconium (Zr) fissile product is produced in the nuclear fuel, part of the Zr element is dissolved in the nuclear fuel matrix, and another part of the Zr element forms simple oxides (ZrO2) with oxygen or complex oxides with Ba, Sr, Cs, Mo, O, etc., that is, "gray phase", which affects the service performance of the nuclear fuel. Therefore, it is necessary to characterize and analyze the fissile product Zr of the nuclear fuel to obtain the concentration and distribution of Zr, which is of great significance for in-depth understanding of the evolution behavior of the fissile product Zr of the nuclear fuel and predicting the performance of the nuclear fuel in the reactor.

[0003] At present, the fissile product Zr of the nuclear fuel is mainly characterized and analyzed by an electron probe (EPMA) at home and abroad, and the content of Zr is obtained by combining with quantitative analysis of the sample. However, there are a variety of fissile nuclides of Zr (such as 90 Zr, 91 Zr, 92 Zr, 93 Zr, 94 Zr, 96 Zr, etc.) in the irradiated nuclear fuel, and EPMA cannot quantitatively analyze the fissile nuclides of Zr, so the content and distribution of the fissile nuclide Zr cannot be obtained. In recent years, a secondary ion mass spectrometer (SIMS) has been applied in the characterization and analysis of the fissile product of the nuclear fuel. Based on SIMS, the depth distribution, isotope abundance and surface distribution of the fissile product of the nuclear fuel can be obtained. However, due to the existence of a large amount of fissile nuclides in the irradiated nuclear fuel, the atomic groups formed by the interaction of these fissile nuclides will form mass spectrum interference to the mass spectrum peak of the fissile nuclide Zr, which significantly increases the difficulty of analyzing the fissile nuclide Zr by SIMS and the accuracy of the quantitative analysis results. SUMMARY

[0004] The purpose of the present application is to solve the above problems, and the fissile nuclide 90 Zr ion implanted cerium dioxide (CeO2) simulation fuel is selected, the primary and secondary light paths of the SIMS are optimized and adjusted, and appropriate analysis parameters (especially the primary beam, the contrast aperture, the field aperture, the scanning area, the entrance slit, the exit slit and the energy slit) are adopted to perform depth profiling and concentration calibration on the fissile nuclide 90 Zr in the CeO2 simulation fuel, so as to obtain the concentration distribution of the fissile nuclide 90 Zr in the depth direction of the CeO2 simulation fuel, and establish the fissile nuclide 90The quantitative analysis method for Zr provides technical support and data support for the characterization and analysis of Zr fission nuclide in irradiated nuclear fuel and the study of fission product behavior.

[0005] Therefore, this invention provides a SIMS-based quantitative analysis method for the fissile nuclide Zr, the method comprising:

[0006] (1) Injection of CeO2 simulated fuel sample onto the surface using an ion accelerator 90 Zr + ion;

[0007] (2) In 90 Zr + A thin layer of gold or platinum is uniformly deposited on the surface of the ion-implanted CeO2 sample.

[0008] (3) Mix Si / Ta standard and 90 Zr + The ion-implanted CeO2 sample is loaded into the sample holder of the SIMS, and the sample holder is loaded into the sample analysis chamber. The secondary and primary optical paths of the SIMS are optimized and adjusted on the Si / Ta standard using the first primary beam current. The second primary beam current, contrast aperture, field aperture, maximum analysis area, scanning area, and energy slit parameters are adjusted and set. The detector electron multiplier and Faraday cup are calibrated.

[0009] (4) Focus the primary ion beam to reduce astigmatism; move the magnetic field to find 90 The secondary ion signal of Zr is then used to calibrate the position of the energy slit, so that... 90 Zr has the strongest secondary ion signal intensity, and the deflection plate is calibrated accordingly.

[0010] (5) Fission nuclides injected into the surface of CeO2 samples by automatic scanning 90 Zr and matrix elements 140 Ce is used for magnetic field calibration to eliminate the effects of other monatomic or group ions. 90 Zr mass spectrometry interference, and then to 90 Zr was analyzed in depth using electron multipliers. 90 Secondary ion signal of Zr 90 After the in-depth analysis of Zr, 140 In-depth analysis of Ce element was performed using Faraday cup collection. 140 The secondary ion signal of Ce element was used to obtain fission nuclides. 90 The curve of secondary ion intensity of Zr as a function of sputtering time;

[0011] (6) Based on fission nuclides 90 The depth corresponding to the peak Zr concentration, 90The secondary ion intensity of Zr was calibrated by measuring the change curve of sputtering time. 90 The curve showing the variation of secondary ion intensity of Zr with sputtering depth is as follows: 140 The secondary ionic strength of Ce is used as a reference, according to 90 Zr + The ion implantation dose, for 90 Concentration calibration was performed using the curve of secondary ion intensity of Zr versus sputtering depth to obtain fissile nuclides. 90 The Zr concentration variation curve with sputtering depth, i.e., the concentration distribution, relative sensitivity factor and detection limit along the depth direction of the CeO2 sample.

[0012] As a preferred embodiment, in the aforementioned SIMS-based quantitative analysis method for the fissile nuclide Zr, the injection energy in step (1) is 400~800 keV. This energy range ensures... 90 Zr + Effective ion implantation into the CeO2 sample surface, forming a controllable depth distribution, is beneficial for utilizing SIMS. 90 In-depth analysis of Zr.

[0013] As a preferred option, in the above-mentioned SIMS-based quantitative analysis method for fission nuclides Zr, the injection temperature in step (1) is room temperature. Room temperature operation avoids thermal damage to the sample, ensures the stability of the CeO2 crystal structure after ion implantation, and prevents high-temperature irradiation from introducing a large number of defects such as vacancies and dislocation loops in the CeO2 sample and affecting the diffusion of Zr, thus affecting the concentration distribution of Zr.

[0014] As a preferred embodiment, in the above-mentioned SIMS-based quantitative analysis method for fissile nuclides Zr, the injection dose in step (1) is 5 × 10⁻⁶. 13 ~1×10 17 ions / cm 2 Dosage selection must match analytical sensitivity and avoid oversaturation effects. Low doses are suitable for trace analysis, while high doses can enhance signal intensity.

[0015] As a preferred embodiment, in the above-mentioned SIMS-based quantitative analysis method for fissile nuclides Zr, step (1) involves injecting... 90 Zr + The peak ion concentration corresponds to a depth of 100–300 nm. This can be achieved by controlling the implantation energy. 90 Zr + The peak ion concentration is located in this depth range, which facilitates the accurate capture of the concentration gradient during SIMS depth profiling.

[0016] As a preferred solution, in the above-mentioned SIMS-based fissile nuclide Zr quantitative analysis method, in step (2), the thickness of the thin layer is 2-30 nm. The gold or platinum thin layer is used to eliminate the charge accumulation effect. The thinner coating layer (2 nm) reduces signal attenuation, and the thicker coating layer (30 nm) is suitable for high beam conditions and ensures uniform surface conductivity.

[0017] As a preferred solution, in the above-mentioned SIMS-based fissile nuclide Zr quantitative analysis method, in step (3), the primary ion source is an oxygen source, and the acceleration voltages of the primary ion beam and the secondary ion beam are +12-15 kV and +5 kV, respectively, which optimizes the sputtering efficiency and secondary ion yield.

[0018] As a preferred solution, in the above-mentioned SIMS-based fissile nuclide Zr quantitative analysis method, in step (3), the first primary beam current is 2-10 nA, which is used for optical path preliminary calibration, and low beam current reduces sample damage.

[0019] As a preferred solution, in the above-mentioned SIMS-based fissile nuclide Zr quantitative analysis method, in step (3), the second primary beam current is adjusted and set to 100-200 nA, which is the analysis beam current. Higher current improves sputtering rate and signal intensity. The contrast aperture is 400 μm or 150 μm, and the field aperture is 750 μm or 400 μm, which controls the beam spot size and analysis area. Large aperture improves the secondary ion intensity of Zr, and small aperture improves the spatial resolution. The maximum analysis area is 150×150 μm 2 or 100×100 μm 2 , and the scanning area is (100×100) μm 2 ~(250×250) μm 2 , which can avoid the interference of the grain size of the CeO2 sample and the arc pit effect of the SIMS sputtering pit on the secondary ion signal of the measured Zr.

[0020] As a preferred solution, in the above-mentioned SIMS-based fissile nuclide Zr quantitative analysis method, in step (3), the energy slit width is 25-100 eV, the entrance slit width is 40-80 μm, and the exit slit width is 80-120 μm, which jointly optimizes the mass resolution and signal intensity.

[0021] In the above-mentioned SIMS-based fissile nuclide Zr quantitative analysis method, in step (3), the mass resolution is 2000-3000 a.m.u, and the electronic gate EGate is 70%-90%.

[0022] As a preferred embodiment, in the step (4), the primary ion beam is focused by adjusting the L4 lens and the stigmators (Stig X, Stig Y and D5 S1) on the CeO2 sample to reduce the astigmatism; the magnetic field is moved to find the secondary ion signal of Zr, then the position of the energy slit is calibrated to maximize the secondary ion signal of Zr, and the deflection plates (DTCA and DTFA) are calibrated. 90 Zr, then the position of the energy slit is calibrated to maximize the secondary ion signal of Zr, and the deflection plates (DTCA and DTFA) are calibrated. 90 Zr, then the position of the energy slit is calibrated to maximize the secondary ion signal of Zr, and the deflection plates (DTCA and DTFA) are calibrated. 90 Zr, then the position of the energy slit is calibrated to maximize the secondary ion signal of Zr, and the deflection plates (DTCA and DTFA) are calibrated.

[0023] Compared with the prior art, the present application has at least the following beneficial effects:

[0024] The present application provides a SIMS-based quantitative analysis method for fissile nuclide Zr, by which the concentration distribution of fissile nuclide Zr in the depth direction of CeO2 simulated fuel, 90 90 Zr, and the relative sensitivity factor and detection limit of Zr. The method can be used for characterization and analysis of fissile nuclide Zr in irradiated nuclear fuel, and the relative sensitivity factor of Zr obtained by the method can be used for concentration calibration of the secondary ion intensity of fissile nuclide Zr in irradiated nuclear fuel at different radial positions (from the center to the edge) along the depth direction, so as to obtain the concentration distribution of fissile nuclide Zr along the radial direction in the irradiated nuclear fuel. 90 Zr, and the relative sensitivity factor and detection limit of Zr. The method can be used for characterization and analysis of fissile nuclide Zr in irradiated nuclear fuel, and the relative sensitivity factor of Zr obtained by the method can be used for concentration calibration of the secondary ion intensity of fissile nuclide Zr in irradiated nuclear fuel at different radial positions (from the center to the edge) along the depth direction, so as to obtain the concentration distribution of fissile nuclide Zr along the radial direction in the irradiated nuclear fuel. 90 Zr along the radial direction.

[0025] The above description is only a summary of the technical scheme of the present application, in order to more clearly understand the technical means of the present application, the specific embodiments of the present application can be implemented according to the content of the specification, and in order to make the above and other purposes, features and advantages of the present application more obvious and easy to understand, the following specific embodiments of the present application are described. BRIEF DESCRIPTION OF DRAWINGS

[0026] Figure 1 The concentration curve of Zr ions in the CeO2 simulated fuel sample of Example 1 is shown. 90 Zr ions in the CeO2 simulated fuel sample of Example 1 is shown.

[0027] Figure 2 The concentration curve of Zr ions in the CeO2 simulated fuel sample of Example 2 is shown. 90 Zr ions in the CeO2 simulated fuel sample of Example 2 is shown. ​

[0028] Figure 3 The CeO2 simulated fuel sample of Example 3 is shown. 90 Concentration curve of Zr ions;

[0029] Figure 4 The CeO2 simulated fuel sample of Example 4 is shown. 90 Concentration curve of Zr ions. Detailed Implementation

[0030] The following description provides numerous specific details to offer a more thorough understanding of the technical solutions provided by this invention. However, it will be apparent to those skilled in the art that the technical solutions provided by this invention can be implemented without one or more of these details.

[0031] In this embodiment of the invention, a method for quantitative analysis of fissile nuclide Zr based on SIMS includes: (1) injecting ion accelerators into the surface of a milled and mechanically polished CeO2 simulated fuel sample at room temperature. 90 Zr + The ion implantation dosage varies in different embodiments; (2) using a coating apparatus in 90 Zr + A thin layer of gold was uniformly deposited on the surface of the ion-implanted CeO2 sample, with varying thicknesses in different embodiments; (3) Si / Ta standard samples and 90 Zr + The ion-implanted CeO2 sample was loaded into the SIMS sample holder, which was then placed into an Airlock. The sample holder was then inserted into the sample analysis chamber via an automated sample introduction system. 2+ The primary ion source, the primary ion beam and the secondary ion beam acceleration voltage are +15kV and +5kV respectively. The secondary optical path (Projection, LCOUP and Transfer) and the primary optical path of SIMS are optimized and adjusted on the Si / Ta standard sample using a first primary beam current of 2~10 nA. The second primary beam current (different in each embodiment), the contrast aperture, the field aperture, the maximum analysis area, the scanning area, the energy slit and other parameters are adjusted and set, and the detector electron multiplier and Faraday cup are calibrated; (4) The primary beam current is different in each embodiment, the energy slit width, the entrance slit width, the exit slit width are different in each embodiment, the quality resolution, the electronic gate EGate are different in each embodiment. On the CeO2 sample, the primary ion beam is focused by adjusting the L4 lens, the astigmatism reducer Stig X, Stig Y and D5 S1, and the moving magnetic field is used to find 90 The secondary ion signal of Zr is then used to calibrate the position of the energy slit, so that... 90Zr has the strongest secondary ion signal, and the deflection plates DTCA and DTFA are calibrated; (5) fissile elements implanted on the surface of the CeO2 sample are scanned automatically 90 Zr and the matrix element 140 Ce is calibrated by a magnetic field, eliminating the influence of other single atom ions or atomic group ions 90 Zr, and then the mass spectrum interference of 90 Zr is analyzed in depth, and the secondary ion signal of 90 Zr is collected by an electron multiplier 90 Zr is analyzed in depth, and the secondary ion signal of 140 Ce is analyzed in depth, and the secondary ion signal of 140 Ce is collected by a Faraday cup 90 Zr, and the depth profile of 90 Zr is calibrated according to the depth corresponding to the peak concentration of 90 Zr, and the depth profile of 90 Zr is obtained according to the secondary ion intensity of 140 Ce, and the depth profile of 90 Zr + ions, and the depth profile of 90 Zr is calibrated according to the secondary ion intensity of 90 Zr, that is, the concentration distribution, relative sensitivity factor and detection limit along the depth direction of the CeO2 sample.

[0032] Example 1

[0033] 90 The implantation energy of Zr ions is 400 keV, and the irradiation dose is 5×10 13 ions / cm 2 ;

[0034] Primary ion beam acceleration voltage: +15 kV, secondary ion beam acceleration voltage: +5 kV, primary beam current: 200 nA, scanning area: 125×125 μm 2 , field aperture: 750 μm, maximum analysis area: 150×150 μm 2 , entrance slit width: 80 μm, exit slit width: 120 μm, mass resolution: 2000 a.m.u, EGate: 90%, energy slit width: 50 eV, and the sample surface is plated with gold to a thickness of 2.5 nm. Figure 1The concentration profile of Zr ions in the CeO2 simulated fuel sample of Example 1 is shown. 90 The concentration profile of Zr ions in the CeO2 simulated fuel sample of Example 1 is shown. 90 The relative sensitivity factor for Zr is 4.366 x 10 22 atom / cm 3 The detection limit is 8.119 x 10 14 atom / cm 3 .

[0035] Example 2

[0036] 90 The Zr ions were implanted at an energy of 400 keV and a dose of 5 x 1015 13 ions / cm 2 ;

[0037] Primary ion beam acceleration voltage: +15 kV, secondary ion beam acceleration voltage: +5 kV, primary beam current: 160 nA, scan area: 125 x 125 μm 2 Contrast aperture: 400 μm, field aperture: 750 μm, maximum analysis area: 150 x 150 μm 2 Inlet slit width: 80 μm, exit slit width: 120 μm, mass resolution: 2000 a.m.u, EGate: 90%, energy slit width: 50 eV, sample surface gold coating thickness: 2.5 nm. Figure 2 The concentration profile of Zr ions in the CeO2 simulated fuel sample of Example 2 is shown. 90 The concentration profile of Zr ions in the CeO2 simulated fuel sample of Example 1 is shown. 90 The relative sensitivity factor for Zr is 4.489 x 10 22 atom / cm 3 The detection limit is 4.626 x 10 14 atom / cm 3 .

[0038] Example 3

[0039] 90 The Zr ions were implanted at an energy of 400 keV and a dose of 2 x 1015 14 ions / cm 2 ;

[0040] Primary ion beam acceleration voltage: +15 kV, secondary ion beam acceleration voltage: +5 kV, primary beam current: 200 nA, scan area: 125 x 125 μm 2 Contrast aperture: 400 μm, field aperture: 750 μm, maximum analysis area: 150 x 150 μm 2Primary Ion Beam Acceleration Voltage: +15 kV, Secondary Ion Beam Acceleration Voltage: +5 kV, Primary Beam Current: 200 nA, Scan Area: 150 x 150 μm Figure 3 The concentration profile of Zr ions in the CeO2 simulated fuel sample of Example 3 is shown in Figure 3. 90 The concentration profile of Zr ions in the CeO2 simulated fuel sample of Example 3 is shown in Figure 3. 90 The relative sensitivity factor for Zr is 2.960 x 10 22 atom / cm 3 The detection limit for Zr is 8.284 x 10 14 atom / cm 3 .

[0041] Example 4

[0042] 90 The concentration profile of Zr ions in the CeO2 simulated fuel sample of Example 4 is shown in Figure 6. 15 ions / cm 2 ;

[0043] Primary Ion Beam Acceleration Voltage: +15 kV, Secondary Ion Beam Acceleration Voltage: +5 kV, Primary Beam Current: 200 nA, Scan Area: 150 x 150 μm 2 Contrast Aperture: 400 μm, Field Aperture: 750 μm, Maximum Analysis Area: 150 x 150 μm 2 Primary Ion Beam Acceleration Voltage: +15 kV, Secondary Ion Beam Acceleration Voltage: +5 kV, Primary Beam Current: 200 nA, Scan Area: 150 x 150 μm Figure 4 The concentration profile of Zr ions in the CeO2 simulated fuel sample of Example 4 is shown in Figure 6. 90 The concentration profile of Zr ions in the CeO2 simulated fuel sample of Example 3 is shown in Figure 3. 90 The relative sensitivity factor for Zr is 2.785 x 10 22 atom / cm 3 The detection limit for Zr is 1.559 x 10 15 atom / cm 3 .

[0044] The above only is the preferred embodiment of the present application, and is not used to limit the present application, for the person skilled in the art, the present application can have various changes and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application, should be included in the protection scope of the present application.

Claims

1. A method for quantitatively analyzing a fissile nuclide Zr based on SIMS, characterized by, The method comprises: (1) CeO2 simulated fuel samples are bombarded with ions using an ion accelerator 90 Zr + ions; (2) In 90 Zr + The ion-implanted CeO2 samples were uniformly coated with a thin layer of gold or platinum on the surface; (3) The Si / Ta standard sample and 90 Zr + The ion-implanted CeO2 sample is loaded into a sample holder of the SIMS, the sample holder is loaded into a sample analysis chamber, the secondary light path and the primary light path of the SIMS are adjusted and optimized on the Si / Ta standard sample by using a first primary beam, the second primary beam, the contrast aperture, the field aperture, the maximum analysis area, the scanning area and the energy slit parameters are adjusted and set, and the detector electron multiplier and the Faraday cup are calibrated. (4) Adjust the L4 lens and the stigmator on the CeO2 sample to focus the primary ion beam and reduce the stigmation. Move the magnetic field to find the secondary ion signal of Zr, then calibrate the position of the energy slit to make the secondary ion signal of Zr the strongest 90 Zr the strongest, and calibrate the deflection plate. 90 Zr the strongest, and calibrate the deflection plate. (5) The fissile nuclides injected on the surface of CeO2 sample by automatic scanning mode 90 Zr and matrix elements 140 Ce for magnetic field calibration, eliminating the influence of other single atom ions or atomic group ions 90 Zr, and then the mass spectrum interference of 90 Zr is analyzed in depth, and the secondary ion signals of 90 Zr are collected by electron multiplier, 90 Zr are analyzed in depth, and the secondary ion signals of 140 Ce are analyzed in depth, and the secondary ion signals of 140 Ce are collected by Faraday cup, 90 The secondary ion intensity of Zr changes with sputtering time. (6) Based on fission nuclides 90 The depth corresponding to the peak Zr concentration, 90 The secondary ion intensity of Zr was calibrated by measuring the change curve of sputtering time. 90 The curve showing the variation of secondary ion intensity of Zr with sputtering depth is as follows: 140 The secondary ionic strength of Ce is used as a reference, according to 90 Zr + The ion implantation dose, for 90 Concentration calibration was performed using the curve of secondary ion intensity of Zr versus sputtering depth to obtain fissile nuclides. 90 The Zr concentration variation curve with sputtering depth, i.e., the concentration distribution, relative sensitivity factor and detection limit along the depth direction of the CeO2 sample.

2. The SIMS-based fissile nuclide Zr quantification method according to claim 1, characterized by, In step (1), the energy injection is 400-800 keV.

3. The SIMS-based fissile nuclide Zr quantitative analysis method according to claim 1, characterized in that, In step (1), the injection temperature is room temperature. In step (1), the implant dose was 5 x 1013ions / cm2 13 1 x 1013ions / cm2 17 ions / cm2 2 .

4. The SIMS-based method of quantifying the fissile nuclide Zr according to claim 1, wherein, In step (1), the injection 90 Zr + The depth corresponding to the ion peak concentration is 100-300 nm.

5. The SIMS-based method of quantifying the fissile nuclide Zr according to claim 1, wherein, In step (2), the thickness of the thin layer is 2-30 nm.

6. The SIMS-based method of quantifying the fissile nuclide Zr according to claim 1, wherein, In step (3), the primary ion source is an oxygen source, and the acceleration voltages of the primary ion beam and the secondary ion beam are +12-15 kV and +5 kV, respectively.

7. The SIMS-based fissile nuclide Zr quantitative analysis method according to claim 1, characterized in that, In step (3), the first primary beam current is 2-10 nA. In step (3), the second primary beam current is adjusted and set to 100-200 nA, the contrast aperture is 400 μm or 150 μm, the field aperture is 750 μm or 400 μm, and the maximum analysis area is 150×150 μm or 100×100 μm 2 . 2 The scanning area is 100×100 μm 2 ~250×250 μm 2 .

8. The SIMS-based method of quantifying the fissile nuclide Zr according to claim 1, wherein, In step (3), the energy slit width is 25-100 eV, the entrance slit width is 40-80 μm, and the exit slit width is 80-120 μm.

9. The SIMS-based method of quantifying the fissile nuclide Zr according to claim 1, wherein, In step (3), the mass resolution is 2000-3000, and the electron gating is 70%-90%.

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