Analytical method and analytical apparatus

Abstract

This provides an analytical method that can accurately correct X-ray spectra. [Solution] The analytical method according to the present invention is an analytical method using an analytical apparatus equipped with multiple wavelength-dispersive X-ray spectrometers, and includes the steps of: obtaining an X-ray spectrum obtained by spectrally analyzing X-rays using a first spectrometer; obtaining information on the time change in the intensity of correction element's X-rays obtained by spectrally analyzing X-rays using a second spectrometer and detecting the X-rays of correction element's X-rays; and correcting the intensity of the X-rays of the target element in the X-ray spectrum based on the information on the time change in the intensity of correction element's X-rays, wherein in the step of correcting the intensity of the X-rays of the target element, information on the intensity of correction element's X-rays detected at the same time as the X-rays of the target element is obtained from the information on the time change in the intensity of correction element's X-rays, and the intensity of the X-rays of the target element is corrected based on the information on the intensity of correction element's X-rays detected at the same time as the X-rays of the target element.

Description

[Technical Field]

[0001] This invention relates to an analytical method and an analytical apparatus. [Background technology]

[0002] Wavelength-dispersive X-ray spectrometers (WDS) perform elemental analysis by spectrally analyzing characteristic X-rays emitted from a sample. Compared to energy-dispersive X-ray spectrometers (EDS), WDS have higher energy resolution and can accurately separate characteristic X-rays with similar energies. Furthermore, WDS have a better signal-to-noise ratio (SNR) than EDS, enabling the detection of trace elements.

[0003] In WDS (Whole-Sea Detector) analysis, X-rays with wavelengths (energies) corresponding to the position of the spectrometer are detected. Therefore, while the sample is irradiated with an electron beam, the spectrometer must be moved a distance corresponding to the wavelength range to be measured. Consequently, WDS cannot detect all elements simultaneously. Therefore, the surface condition or composition of the sample may change between the start and end of the measurement.

[0004] For example, contamination primarily composed of carbon can increase the signal level of carbon. Furthermore, in samples containing alkali metals, such as soda-lime glass, or soft materials like polymers, biological membranes, and biomolecules, elements that are susceptible to electron beam damage may not be detected, or may be detected at lower concentrations than they should be.

[0005] To address such problems, for example, Patent Document 1 discloses a quantitative analysis method comprising the steps of: measuring the effect of electron beam irradiation time required for carbon analysis on the detection X-ray intensity during qualitative analysis of steel, and creating and registering an analysis measurement time effect curve; and performing a qualitative analysis of steel, and, according to the analysis measurement time required for carbon analysis, performing a quantitative correction on the quantitative analysis result of carbon based on the energy spectral intensity obtained from the qualitative analysis result, based on the analysis measurement time effect curve that was registered in advance. [Prior art documents] [Patent Documents]

[0006] [Patent Document 1] Japanese Patent Publication No. 2007-178445 [Overview of the Initiative] [Problems that the invention aims to solve]

[0007] As described above, in the method disclosed in Patent Document 1, the effect of the electron beam irradiation time required for carbon analysis on the detected X-ray intensity is measured in advance to create an analysis measurement time effect curve, and the created analysis measurement time effect curve is used to correct the quantitative analysis results.

[0008] However, in actual measurements, the X-ray intensity of carbon may not change according to the pre-created analysis time-effect curve. Therefore, the method disclosed in Patent Document 1 may not be able to accurately correct the quantitative analysis results. [Means for solving the problem]

[0009] One aspect of the analytical method according to the present invention is: An analytical method using an analytical instrument equipped with multiple wavelength-dispersive X-ray spectrometers, The sample is irradiated with an electron beam, and the X-rays emitted from the sample are divided into the plurality of wavelength-dispersive X-ray components. A step of obtaining an X-ray spectrum obtained by spectral analysis using at least one first spectrometer among the optical instruments, A step of obtaining information on the time change in the intensity of the X-rays of the correction element, obtained by irradiating the sample with an electron beam, spectrally analyzing the X-rays emitted from the sample using at least one second spectrometer among the plurality of wavelength-dispersive X-ray spectrometers, and detecting the X-rays of the correction element. A step of correcting the X-ray intensity of the element to be analyzed in the X-ray spectrum based on information on the time evolution of the X-ray intensity of the correction element, Includes, In the step of correcting the X-ray intensity of the element to be analyzed, From the time-varying information of the X-ray intensity of the correction element, information on the intensity of the X-ray of the correction element detected at the same timing as the X-ray of the element to be analyzed is obtained. Based on the intensity information of the X-rays of the correction element detected at the same time as the X-rays of the element to be analyzed, the intensity of the X-rays of the element to be analyzed is corrected.

[0010] In this type of analysis method, the intensity of the X-rays of the target element is corrected based on information about the intensity of X-rays of a correction element detected at the same time as the X-rays of the target element, thus enabling accurate correction of the X-ray intensity of the target element.

[0011] One aspect of the analytical apparatus according to the present invention is: An electron optical system that irradiates a sample with an electron beam, Multiple wavelength-dispersive X-ray spectrometers for spectrally analyzing the X-rays emitted from the sample, A processing unit that corrects the intensity of X-rays of the element to be analyzed in the X-ray spectrum, Includes, The aforementioned processing unit, A process to obtain the X-ray spectrum obtained by spectrally analyzing the X-rays emitted from the sample using at least one first spectrometer among the plurality of wavelength-dispersive X-ray spectrometers, a process of acquiring information on a temporal change in the intensity of X-rays of the correction element, which is obtained by spectroscopically separating X-rays emitted from the sample using at least one second spectrometer among said plurality of wavelength-dispersive X-ray spectrometers to detect the X-rays of the correction element; a process of correcting the intensity of X-rays of the analysis target element based on the information on the temporal change in the intensity of X-rays of the correction element; wherein in the process of correcting the intensity of X-rays of the analysis target element, information on the intensity of X-rays of the correction element detected at the same timing as the X-rays of the analysis target element is acquired from the information on the temporal change in the intensity of X-rays of the correction element, and the intensity of X-rays of the analysis target element is corrected based on the information on the intensity of X-rays of the correction element detected at the same timing as the X-rays of the analysis target element.

[0012] In such an analyzer, a processing unit corrects the intensity of X-rays of the analysis target element based on the information on the intensity of X-rays of the correction element detected at the same timing as the X-rays of the analysis target element, so the intensity of X-rays of the analysis target element can be corrected accurately. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] [Figure 1] A diagram showing an example of the configuration of an analyzer. [Figure 2] A diagram showing an example of the configuration of an analyzer. [Figure 3] A diagram for explaining a method of acquiring a spectrum in WDS. [Figure 4] A diagram for explaining map analysis in WDS. [Figure 5] A diagram for explaining spectral imaging. [Figure 6] A flowchart showing an example of a method for acquiring a spectral map. [Figure 7] A reflected electron image of a sample. [Figure 8] A graph showing the temporal change in the count number of carbon. [Figure 9] A diagram showing the temporal change of a carbon map. [Figure 10] A graph showing the increase curve of carbon in each region. [Figure 11] A diagram illustrating the method for correcting spectral maps. [Figure 12] A flowchart illustrating an example of a method for correcting X-ray intensity. [Figure 13] A diagram illustrating the method for specifying the correction area. [Figure 14] A flowchart illustrating an example of the processing steps in the processing unit. [Figure 15] A figure showing an example of displaying the X-ray spectrum and the carbon increase curve measured simultaneously with the X-ray spectrum. [Modes for carrying out the invention]

[0014] Preferred embodiments of the present invention will be described in detail below with reference to the drawings. The embodiments described below are not intended to unduly limit the scope of the present invention as described in the claims. Furthermore, not all of the configurations described below are essential components of the present invention.

[0015] 1. Analyzer First, an analytical apparatus used in the analytical method according to one embodiment of the present invention will be described with reference to the drawings. Figures 1 and 2 show an example of the configuration of the analytical apparatus 100 used in the analytical method according to this embodiment. The analytical apparatus 100 is a scanning electron microscope equipped with multiple wavelength-dispersive X-ray spectrometers (WDS). The analytical apparatus 100 may also be an electron probe microanalyzer (EPMA) equipped with multiple WDS.

[0016] As shown in Figures 1 and 2, the analyzer 100 includes an electron optical system 10, a sample stage 20, an electron detector 30, WDS50a, WDS50b, WDS50c, WDS50d, WDS50e, a processing unit 60, an operation unit 70, a display unit 72, and a storage unit 74. Note that in Figure 2, for convenience, only the electron optical system 10, WDS50a, WDS50b, WDS50c, WDS50d, and WDS50e are shown.

[0017] The electron optical system 10 irradiates the sample S with an electron beam EB. The electron optical system 10 includes an electron gun 12, a focusing lens 14, a deflector 16, and an objective lens 18.

[0018] The electron gun 12 emits an electron beam EB. The electron gun 12 emits an electron beam EB, accelerated by a predetermined acceleration voltage, toward the sample S.

[0019] The focusing lens 14 focuses the electron beam EB emitted from the electron gun 12. The deflector 16 deflects the electron beam EB two-dimensionally. The deflector 16 allows the electron beam EB to scan the sample S. The objective lens 18 focuses the electron beam EB on the sample S. By focusing the electron beam EB with the focusing lens 14 and the objective lens 18, an electron probe can be formed.

[0020] The sample stage 20 supports the sample S. The sample S is placed on the sample stage 20. Although not shown in the diagram, the sample stage 20 is equipped with a movement mechanism for moving the sample S. For example, by moving the sample S on the sample stage 20, the sample S can be scanned with an electron beam EB.

[0021] The electron detector 30 is a detector for detecting electrons emitted from the sample S. By scanning the sample S with an electron beam EB and detecting the electrons emitted from the sample S with the electron detector 30, a scanning electron microscope (SEM) image can be obtained. The electron detector 30 may be a backscattered electron detector for detecting backscattered electrons, or a secondary electron detector for detecting secondary electrons. By detecting backscattered electrons with the electron detector 30, a backscattered electron image can be obtained. Furthermore, A secondary electron image can be obtained by detecting secondary electrons with the electron detector 30.

[0022] The analyzer 100 is equipped with five WDSs (WDS50a, WDS50b, WDS50c, WDS50d, and WDS50e). The number of WDSs that the analyzer 100 may be equipped with is not particularly limited.

[0023] The WDS50a includes a spectroscopic element 52a and an X-ray detector 54a. In the WDS50a, characteristic X-rays generated from the sample S are spectrally analyzed by the spectroscopic element 52a, and the spectrally analyzed X-rays are detected by the X-ray detector 54a.

[0024] The spectroscopic element 52a is, for example, a spectroscopic crystal used to perform spectroscopy using the diffraction phenomenon of X-rays. The WDS50a is equipped with multiple spectroscopic elements 52a with different interplanar spacings. That is, the multiple spectroscopic elements 52a have different spectral wavelength ranges. Examples of spectroscopic elements 52a include PET (pentaerythritol), LiF (lithium fluoride), TAP (thallium acid phthalate), and STE (stearate). The X-ray detector 54a detects the characteristic X-rays spectrally separated by the spectroscopic elements 52a.

[0025] The WDS50a includes a drive unit for moving the spectroscopic element 52a and the X-ray detector 54a. The drive unit moves the spectroscopic element 52a and the X-ray detector 54a, for example, by motor drive. This allows the spectroscopic element 52a and the X-ray detector 54a to be positioned in the desired location. The WDS50a can detect X-rays of a wavelength (energy) corresponding to the position of the spectroscopic element 52a.

[0026] As shown in Figure 2, the analyzer 100 is equipped with WDS50a, WDS50b, WDS50c, WDS50d, and WDS50e. WDS50b, WDS50c, WDS50d, and WDS50e have the same configuration as WDS50a. WDS50b has multiple spectroscopic elements 52b and an X-ray detector 54b. Although not shown in the figure, WDS50c, WDS50d, and WDS50e each also have multiple spectroscopic elements and an X-ray detector. Since the analyzer 100 is equipped with five WDSs, it can perform five measurements simultaneously.

[0027] The operation unit 70 acquires operation signals in response to user operations and sends them to the processing unit 60. The operation unit 70 may be, for example, a button, a key, a touch panel display, or a microphone.

[0028] The display unit 72 displays the image generated by the processing unit 60. The display unit 72 is a display such as an LCD (liquid crystal display).

[0029] The memory unit 74 stores programs and data for the processing unit 60 to perform various calculation and control processes. The memory unit 74 is also used as a work area for the processing unit 60. Examples of memory units 74 include RAM (Random Access Memory), ROM (Read Only Memory), and hard disks.

[0030] The functions of the processing unit 60 can be realized by executing programs stored in the memory unit 74 using hardware such as various processors (CPU (Central Processing Unit), DSP (Digital Signal Processor), etc.). The processing unit 60 performs processing to control each part that makes up the analytical device 100. For example, the processing unit 60 controls the electron optical system 10 and WDS 50a, 50b, 50c, 50d, and 50e. The processing unit 60 also performs processing to correct the X-ray spectrum. Furthermore, the processing unit 60 performs processing to display the X-ray spectrum and correction data on the display unit 72.

[0031] The processing unit 60 includes a control unit 62 that controls each part of the analyzer 100, a calculation unit 64 that performs processing to correct the X-ray spectrum, and a display control unit 66 that displays information on the time change of the X-ray spectrum and the X-ray intensity of the correction element. Details of the control unit 62, the calculation unit 64, and the display control unit 66 will be described later.

[0032] 2. Operation of the analytical instrument 2.1. Point analysis Figure 3 is a diagram illustrating the method for acquiring spectra using the WDS50a.

[0033] In the WDS50a, the analysis point (electron beam irradiation position) on the sample S, the spectrometer 52a, and the X-ray detector 54a are arranged on the Rowland circle to satisfy Bragg's law for focusing conditions. The spectrometer 52a moves along a straight line inclined by an extraction angle φ from the analysis point. The X-ray detector 54a also moves along with the movement of the spectrometer 52a. The distance between the analysis point and the spectrometer 52a is equal to the distance between the spectrometer 52a and the X-ray detector 54a.

[0034] Here, if the position of the spectrometer 52a (spectroscopic position L) is changed while the position of the sample S (analysis point) is fixed, the incident angle θ of X-rays on the spectrometer 52a changes. The spectral position L is expressed as the distance between the sample S (analysis point) and the spectrometer 52a.

[0035] In the example shown in FIG. 3, the spectroscopic element 52a is moved from a spectroscopic position L1 where the distance between the sample S and the spectroscopic element 52a is L1 to a spectroscopic position L2 where the distance between the sample S and the spectroscopic element 52a is L2 (L1 < L2). Accordingly, the incident angle θ is changed from θ1 to θ2 (θ1 < θ2).

[0036] According to Bragg's law, changing the incident angle θ changes the energy (wavelength) of X-rays detected by the X-ray detector 54a. Therefore, by fixing the position of the sample S and changing the spectroscopic position L, an X-ray spectrum (hereinafter, also simply referred to as "spectrum") in which the horizontal axis represents energy (wavelength or spectroscopic position L) and the vertical axis represents X-ray intensity can be obtained.

[0037] 2.2. Map analysis (surface analysis) FIG. 4 is a diagram for explaining map analysis in WDS 50A.

[0038] When acquiring map data representing an intensity distribution for a specific element, that is, characteristic X-rays of a specific energy, the sample S is scanned with an electron beam EB while the spectroscopic position L is fixed. At this time, the spectroscopic element 52a is fixed at the spectroscopic position L corresponding to the energy of the characteristic X-ray to be analyzed. By scanning the sample S with the electron beam EB while the spectroscopic position L is fixed in this manner, X-ray intensity information can be obtained at each analysis point on the sample S. Note that scanning of the sample S with the electron beam EB can be performed by beam scanning or stage scanning.

[0039] Through map analysis, map data in which positions on the sample S are associated with X-ray intensities of specific energy can be obtained. In the map data, the coordinates (position) of each pixel correspond to a position on the sample S. The X-ray intensity information obtained at each analysis point is stored in each pixel.

[0040] Element distribution information can be obtained from the map data obtained as a result of map analysis.

[0041] 2.3. Spectral Imaging Figure 5 is a diagram illustrating spectral imaging.

[0042] Spectral imaging is a technique for obtaining a spectral map (SM). The spectral map (SM) is a map that associates the position on a sample (S) with the spectrum.

[0043] In spectral imaging, for example, map analysis is performed by fixing the spectral position L and acquiring map data, and then repeating this process while changing the spectral position L to acquire multiple map data sets. A spectral map SM is then generated based on the multiple map data sets that have been acquired.

[0044] Figure 6 is a flowchart showing an example of a method for obtaining a spectral map (SM).

[0045] First, a map analysis is performed on sample S at spectral position L1, and the map data M is generated. L1 Obtain (step S10).

[0046] Specifically, the spectral position L is fixed at spectral position L1, and a map analysis is performed on the sample S. This generates map data M. L1 Map data M can be obtained. L1 The coordinates of each pixel are expressed in XY coordinates. Also, map data M L1 Each pixel stores information about the intensity of X-rays at the energy corresponding to the spectral position L1, obtained at the analysis point corresponding to the coordinates of each pixel.

[0047] Next, the spectroscopic element 52a is moved by a predetermined distance (step S20). This changes the spectral position L from spectral position L1 to spectral position L2. The interval at which the position of the spectroscopic element 52a is changed is, for example, constant. That is, the distance between spectral position L1 and spectral position L2 is equal to the distance between spectral position L2 and spectral position L3. The interval at which the position of the spectroscopic element 52a is changed can be changed as appropriate.

[0048] Next, map analysis is performed on the sample S at the spectral position L2, to obtain map data M L2 (step S30).

[0049] Specifically, the spectral position L is fixed at the spectral position L2, and map analysis is performed on the sample S. Thus, map data M L2 can be obtained. For each pixel of the map data M L2 , information about the intensity of X-rays having energy corresponding to the spectral position L2 is stored.

[0050] Next, the map data M L1 and the map data M L2 are combined (step S40).

[0051] X-ray intensity information is extracted from each corresponding pixel of the map data M L1 and the map data M L2 to generate a single piece of map data, whereby a spectral map can be created. Here, each pixel of the spectral map stores spectral data including X-ray intensity information at the spectral position L1 and X-ray intensity at the spectral position L2.

[0052] Step S20 of moving the spectroscopic element 52a, step S30 of performing map analysis, and step S40 of combining map data are repeated to obtain map data M L3 , map data M L4 , ..., map data M LN . When N pieces of map data are obtained (Yes in step S50), the spectral imaging is ended.

[0053] As shown in FIG. 5, each pixel constituting the spectral map SM stores spectral data including X-ray intensity information at N mutually different spectral positions L (spectral position L1, spectral position L2, ..., spectral position L N ). In the example shown in FIG. 5, the horizontal axis of the spectrum represents the spectral position L, but the horizontal axis of the spectrum may also represent the wavelength or energy of X-rays.

[0054] Since the analyzer 100 is equipped with five WDSs, it can acquire five spectral maps SM simultaneously.

[0055] 3. Analysis method 3.1. Analysis Flow The analytical method according to this embodiment includes the steps of: obtaining a spectrum obtained by irradiating a sample S with an electron beam EB and spectrally analyzing the X-rays emitted from the sample S using a WDS50a; obtaining information on the time evolution of the intensity of X-rays of correction elements obtained by irradiating a sample S with an electron beam EB and spectrally analyzing the X-rays emitted from the sample S using a WDS50b and detecting the X-rays of correction elements; and correcting the intensity of the X-rays of the analyte element in the spectrum based on the information on the time evolution of the intensity of X-rays of correction elements.

[0056] 3.2. Acquisition of X-ray spectra The analytical method according to this embodiment involves irradiating a sample S with an electron beam EB and obtaining a spectrum by spectrally analyzing the X-rays emitted from the sample S using a WDS50a. For example, in the analytical device 100, a spectrum can be obtained by performing point analysis using the WDS50a. Alternatively, in the analytical device 100, a spectrum can be obtained by performing spectral imaging using the WDS50a.

[0057] Furthermore, the WDS used to acquire the spectrum is not limited to the WDS50a; any of the WDS50b, WDS50c, WDS50d, or WDS50e may be used. Multiple WDSs may also be used to acquire the spectrum.

[0058] 3.3. Information on the time evolution of X-ray intensity of correction elements In the spectroscopic method according to this embodiment, an electron beam EB is irradiated onto a sample S, and the X-rays emitted from the sample S are spectrally analyzed using a WDS50b to detect the X-rays of the correction element, thereby obtaining information on the time change in the intensity of the X-rays of the correction element.

[0059] Furthermore, the WDS used for measurements to obtain information on the time evolution of the X-ray intensity of the correction elements is not particularly limited, as long as it is not the WDS used to obtain the spectrum described above. For example, if there are multiple correction elements, multiple WDSs may be used.

[0060] The time evolution of the X-ray intensity of the correction element is measured simultaneously with the measurement for spectrum acquisition. For example, when acquiring a spectral map by spectral imaging using WDS50a, the time evolution of the X-ray intensity of the correction element is measured by performing map analysis using WDS50b simultaneously with spectral imaging using WDS50a.

[0061] For example, in WDS50a, map analysis is performed by fixing the position of the spectrometer 52a and acquiring map data, and this process is repeated while changing the position of the spectrometer 52a to acquire multiple map data sets. A spectral map is then generated based on these acquired map data sets. Similarly, in WDS50b, map analysis is performed by fixing the position of the spectrometer 52a and acquiring map data, and multiple map data sets are acquired. Data on the time evolution of the X-ray intensity of the correction element is then generated based on these acquired map data sets. Since spectral imaging with WDS50a and map analysis with WDS50b are performed simultaneously, the number of map analyses performed with WDS50a and WDS50b are equal. The following describes the measurement of the time evolution of the X-ray intensity of the correction element when the correction element is carbon.

[0062] Figure 7 shows an example of a backscattered electron image of sample S. As shown in Figure 7, it can be seen that multiple phases exist in sample S. WDS50b was used for this sample S as a correction element. The time evolution of the carbon X-ray intensity is measured. Here, the position of the spectrometer 52b of the WDS50b is fixed to a position where C-Kα rays can be detected, and map analysis is performed.

[0063] Figure 8 is a graph showing the time evolution of carbon count (X-ray intensity). Figure 8 is the result of a map analysis of the entire field of view of sample S shown in Figure 7. In Figure 8, the X-ray count (intensity) is plotted on the vertical axis, and the time when the X-rays were detected is plotted on the horizontal axis, representing the X-ray intensity measured by the map analysis as a graph.

[0064] As shown in Figure 8, the carbon count increases with the passage of analysis time. This is because carbon-based contaminants accumulate on the sample S due to electron beam irradiation. The carbon increase curve with respect to analysis time shown in Figure 8 is used to correct the spectrum as information on the time change in the intensity of the correction element's X-rays.

[0065] Figure 9 shows the time evolution of the carbon map. Map A in Figure 9 is the map obtained at time Ta in the graph shown in Figure 8, Map B is the map obtained at time Tb, and Map C is the map obtained at time Tc.

[0066] As shown in Figure 9, the carbon count is higher in Map B than in Map A, and higher in Map C than in Map B. Thus, the results of the map analysis shown in Figure 9 also show that the carbon count increases with the progress of the analysis time. Furthermore, the results of the map analysis shown in Figure 9 show that the intensity distribution of carbon is not uniform.

[0067] Figure 10 is a graph showing the carbon increase curves in region S1, region S2, and region S3, as shown in Figure 7.

[0068] As shown in Figure 10, the rate of increase in carbon counts relative to analysis time differs for each region. Therefore, the carbon increase curve differs for each region. The carbon increase curves for each region shown in Figure 10 are used to correct the spectra obtained in each region as information on the time evolution of the X-ray intensity of the correction element in each region. For example, the carbon increase curve in region S1 shown in Figure 10 is used to correct the spectrum obtained in region S1. This allows for more accurate spectrum correction. Similarly, when correcting the spectrum obtained in region S2, the carbon increase curve in region S2 shown in Figure 10 is used, and when correcting the spectrum obtained in region S3, the carbon increase curve in region S3 shown in Figure 10 is used. In this way, by performing map analysis and measuring the time evolution of the X-ray intensity of the correction element, information on the time evolution of the X-ray intensity of the correction element can be obtained for each region.

[0069] 3.4. Correction In the analysis method according to this embodiment, the intensity of the X-rays of the target element in the spectrum is corrected based on information about the time evolution of the X-ray intensity of the correction element. Furthermore, in the step of correcting the intensity of the X-rays of the target element, information about the intensity of the correction element's X-rays detected at the same time as the X-rays of the target element is obtained from the information about the time evolution of the correction element's X-ray intensity, and the intensity of the X-rays of the target element is corrected based on the information about the intensity of the correction element's X-rays detected at the same time as the X-rays of the target element.

[0070] Here, the correction of X-ray intensity includes correcting the X-ray intensity expressed in the spectrum, such as the X-ray count or peak size, and correcting the concentration of the analyte element calculated from the X-ray intensity expressed in the spectrum, such as the X-ray count or peak size.

[0071] Figure 11 is a diagram illustrating the method for correcting the spectral map. Figure 11 shows an example of a spectrum stored in the spectral map and a spectrum measured simultaneously with spectral imaging. An example of the increasing carbon content curve is shown in the figure.

[0072] The spectral map was obtained using the WDS50a by performing the spectral imaging described above. Specifically, the spectral map was obtained by performing a map analysis for each wavelength and combining the map data for each wavelength. In this process, the spectroscopic element 52a of the WDS50a was moved from the short wavelength side to the long wavelength side to perform the map analysis for each wavelength.

[0073] The carbon increase curve shown in Figure 11 was obtained by performing the map analysis described above using WDS50b. Specifically, with WDS50b, the position of the spectroscopic element 52b was fixed, and carbon X-rays were detected.

[0074] Spectral imaging using WDS50a and map analysis using WDS50b are performed simultaneously. Therefore, wavelength (the horizontal axis of the spectrum) and time (the horizontal axis of the graph showing the change in carbon count over time) correspond one-to-one. Consequently, information on the intensity of carbon X-rays when the X-rays of the analyte are detected can be obtained from the carbon increase curve.

[0075] For example, the carbon count curve allows us to determine the carbon count at the time when the peak of the analyte element in the spectrum measured using WDS50a was detected. Therefore, the carbon count detected at the same time as the peak of the analyte element can be used to correct the X-ray intensity (peak size) of the analyte element. In other words, it is possible to estimate how much the peak of the analyte element has been attenuated due to contamination mainly composed of carbon.

[0076] For example, in the example shown in Figure 11, the position of the Ti peak in the spectrum corresponds to time T1 in the graph of the time evolution of the carbon count. That is, the carbon count at time T1 is the carbon X-ray intensity detected at the same time as the Ti X-ray. Similarly, the position of the Si peak corresponds to time T2 in the graph of the time evolution of the carbon count. That is, the carbon count at time T2 is the carbon X-ray intensity detected at the same time as the Si X-ray. Since the carbon count at time T2 is higher than the carbon count at time T1, it can be inferred that the Si peak is attenuated more than the Ti peak.

[0077] Figure 12 is a flowchart illustrating an example of a method for correcting X-ray intensity in a spectral map. Here, we will explain how to correct the spectrum shown in Figure 11 using the carbon increase curve shown in Figure 11.

[0078] First, the correction region is specified in sample S (step S100). Figure 13 is a diagram illustrating the method for specifying the correction region.

[0079] As shown in Figure 13, the correction region can be specified by specifying a range of contrast values ​​for the backscattered electron image. This makes it easy to specify phases with complex shapes or phases that exist in discrete locations as the correction region. Note that the method for specifying the correction region is not limited to methods using electron microscope images such as backscattered electron images. For example, the correction region may be specified by specifying a range of X-ray counts in the element map obtained by map analysis. Alternatively, the region may be specified by the user drawing a shape of any shape on the electron microscope image or element map.

[0080] Next, for each pixel within the correction region, the change in the carbon count from the initial value is calculated (step S102). In the example shown in Figure 11, the carbon count at time T0 of the graph is used as the initial value, and the carbon count at the time the analyte element was detected is calculated relative to this initial value. This calculates the change in the carbon count. For example, if the element being analyzed is Ti, the change in the carbon count from time T0 to time T1 is calculated. Similarly, if the element being analyzed is Si, the change in the carbon count from time T0 to time T2 is calculated.

[0081] Next, based on the calculated change in carbon, the concentration of carbon at the time the analyte was detected is determined (step S104). The conversion from the change in carbon to the carbon concentration may be performed using measurement data of a standard sample measured in advance, or using a quantitative calibration curve stored in a database.

[0082] Next, the intensity of the X-rays of the analyte is corrected based on the carbon concentration information at the time the analyte was detected (step S106).

[0083] Specifically, based on information about the carbon concentration at the time the target element was detected, it is assumed that carbon-based deposits (contaminations) are attached to the sample surface with a thickness proportional to the carbon concentration, and the attenuation of the X-ray intensity of the target element is calculated. The attenuation of X-ray intensity according to the thickness of the deposit may be calculated from measurement data of a standard sample acquired in advance, or it may be calculated by simulation. The thickness of the deposit is calculated from the carbon concentration, and the attenuation of the X-ray intensity of the target element is calculated from the thickness of the deposit. As a result, the X-ray intensity of the target element can be corrected.

[0084] Furthermore, by applying the above corrections to the various elements detected in the correction region and performing quantitative calculations, and by including the carbon concentration at the start of measurement time T0 as the carbon concentration contained in the sample in these quantitative results, the composition of the sample in the correction region can be calculated.

[0085] Through the above process, the intensity of the X-rays of the element to be analyzed can be corrected.

[0086] The above explanation described the case where the count of correction elements increases over time, but the same correction can be applied to the case where the count of correction elements decreases over time.

[0087] For example, alkali metals are susceptible to damage from electron beams, so when measuring a sample containing alkali metals using WDS, the alkali metals that should be present may not be detected, or may be detected at a lower concentration than they should be. Below, we will describe an example in which the correction method shown in Figure 12 above is applied when the correction element is sodium contained in the sample.

[0088] First, a correction region is specified for sample S (step S100), and the change in sodium count is calculated for each pixel within the correction region from the initial value (step S102). Next, based on the calculated change in sodium, the concentration of sodium at the time the analyte was measured is determined (step S104).

[0089] Here, we assume that the relative abundance of other elements within the correction region increases by the amount of the decrease in sodium concentration. The original concentration of sodium can be calculated from the sodium concentration at the start of measurement time T0. Therefore, in the correction region, the sodium concentration contained in the sample is taken as the sodium concentration at the start of measurement time T0, and the concentrations of other elements within the correction region are corrected accordingly. This allows us to obtain compositional information for the correction region.

[0090] The above describes the correction of spectra in spectral maps, but spectra obtained by point analysis can also be corrected in the same way. Furthermore, the above describes the case where only one correction element is used, but multiple correction elements may be set. In this case, the above correction should be applied to each of the multiple correction elements.

[0091] 4. Processing of the Processing Unit Figure 14 is a flowchart showing an example of the processing in the processing unit 60.

[0092] The control unit 62 determines whether the user has given an instruction to start measuring the spectrum (measurement start instruction) (step S200), and waits until the measurement start instruction is given (No. in step S200). The control unit 62 determines that the user has given a measurement start instruction, for example, when the measurement start button is pressed or when a measurement disclosure instruction is input from an input device or the like.

[0093] If the control unit 62 determines that the user has given a measurement start command (Yes in step S200), it starts the measurement to acquire the spectrum (step S202).

[0094] The control unit 62 moves the spectroscopic element 52a of the WDS 50a to a position where a predetermined wavelength within the spectral wavelength range can be detected, and fixes the spectroscopic element 52b of the WDS 50b to a position where X-rays of the correction element can be detected (step S204).

[0095] The memory unit 74 has information about the wavelength range of the spectrum stored in advance, and the control unit 62, for example, first moves the spectroscopic element 52a of the WDS50a to a position where it can detect the shortest wavelength X-rays within the wavelength range of the spectrum. The control unit 62 also fixes the spectroscopic element 52b of the WDS50b to a position where it can detect the X-rays of the correction element, based on the information of the correction element specified by the user.

[0096] The control unit 62 instructs the electron optical system 10 to irradiate the sample S with an electron beam EB (step S206). For example, when performing point analysis, the control unit 62 instructs the electron optical system 10 to irradiate a specified analysis point on the sample S with the electron beam EB. Alternatively, for example, when performing spectral imaging, the control unit 62 instructs the electron optical system 10 to scan a specified area of ​​the sample S with the electron beam EB.

[0097] When a sample S is irradiated with an electron beam EB, X-rays are emitted from the sample S. In WDS50a, X-rays of a predetermined wavelength are extracted from the X-rays emitted from the sample S using the spectroscopic element 52a and detected by the X-ray detector 54a. Simultaneously, in WDS50b, X-rays of correction elements are extracted from the X-rays emitted from the sample S using the spectroscopic element 52b and detected by the X-ray detector 54b. Therefore, WDS50a outputs intensity data of X-rays of a predetermined wavelength. In addition, WDS50b outputs intensity data of X-rays of correction elements.

[0098] Thus, the analyzer 100 uses WDS50a to detect X-rays of a predetermined wavelength for the spectrum and WDS50b to detect X-rays of correction elements, allowing for simultaneous detection of X-rays of a predetermined wavelength for the spectrum and X-rays of correction elements.

[0099] The calculation unit 64 acquires intensity data of X-rays of a predetermined wavelength output from WDS50a and intensity data of X-rays of correction elements output from WDS50b (step S208).

[0100] The control unit 62 determines whether or not measurements have been taken for all wavelengths within the spectral wavelength range (step S210).

[0101] For example, the control unit 62 obtains information on the longest wavelength within the spectral wavelength range from the spectral wavelength range information stored in the memory unit 74, and compares this longest wavelength information with a predetermined wavelength detected by the WDS 50a. The control unit 62 determines that the predetermined wavelength is the wavelength of the spectral wave. Measurements are considered to have been performed for all wavelengths if the value is greater than or equal to the value of the longest wavelength within the long range.

[0102] If the control unit 62 determines that measurements have not been performed for all wavelengths (No. in step S210), it returns to step S204 and moves the spectroscopic element 52a of WDS50a to a position where a predetermined wavelength within the spectral wavelength range can be detected, and fixes the spectroscopic element 52b of WDS50b to a position where X-rays of the correction element can be detected (step S204).

[0103] The control unit 62 moves, for example, the spectroscopic element 52a of the WDS50a by a predetermined distance. This changes the wavelength of the X-rays detected by the WDS50a by a value corresponding to the predetermined distance. At this time, the control unit 62 does not move the spectroscopic element 52b of the WDS50b. Therefore, the spectroscopic element 52b of the WDS50b maintains a position where it can detect X-rays of the correction element.

[0104] The control unit 62 causes the electron optical system 10 to irradiate the sample S with an electron beam EB (step S206), and the calculation unit 64 acquires intensity data of X-rays of a predetermined wavelength output from WDS50a and intensity data of X-rays of correction elements output from WDS50b (step S208).

[0105] The control unit 62 and the calculation unit 64 repeat the processes of steps S204, S206, S208, and S210 until it is determined that measurements have been taken for all wavelengths in the spectral wavelength range.

[0106] If the control unit 62 determines that measurements have been performed for all wavelengths (Yes in step S210), it instructs the electron optical system 10 to stop irradiating the sample S with the electron beam EB, and terminates the measurement (step S212). As a result of the measurement, spectral data and information on the time evolution of the X-ray intensity of the correction element can be obtained. For example, if spectral imaging is performed, a spectral map is obtained as spectral data.

[0107] The calculation unit 64 corrects the intensity of the X-rays of the analyte element in the spectrum based on information about the time evolution of the X-ray intensity of the correction element. Specifically, as explained in "3.4. Correction", the calculation unit 64 obtains information about the intensity of the correction element's X-rays detected at the same time as the analyte element's X-rays from the information about the time evolution of the correction element's X-ray intensity (step S214). Next, the calculation unit 64 corrects the intensity of the analyte element's X-rays based on information about the intensity of the correction element's X-rays detected at the same time as the analyte element's X-rays (step S216). For example, the calculation unit 64 corrects all elements detected by WDS50a as analyte elements to determine the composition of the sample S.

[0108] The processing unit 60 corrects the spectrum and then terminates the process. While the above description explains the case where the processing unit 60 performs the processing from measurement to correction, the user may manually perform at least some of the above processes.

[0109] 5.Display Figure 15 shows an example of a spectrum and a display of the carbon increase curve measured simultaneously with the spectrum.

[0110] As shown in Figure 15, the display control unit 66 displays the spectrum and the carbon increase curve measured simultaneously with the spectrum on the display unit 72. In this case, the horizontal axis is the time axis. This makes it possible to clearly display the peaks of each element in the spectrum and the intensity of carbon X-rays detected at the same time as those peaks.

[0111] Furthermore, as shown in Figure 11, the display control unit 66 may display the spectrum and the carbon increase curve measured simultaneously with the spectrum side by side on the display unit 72.

[0112] Furthermore, the display control unit 66 may highlight the specified correction area, as shown in Figure 13. For example, as shown in Figure 13, the display control unit 66 may draw lines on the contour of the specified correction area on the sample image to highlight the boundary of the correction area. Although not shown, the display control unit 66 may also hatch the specified correction area on the sample image or fill in the correction area.

[0113] 6. Effects The analytical method according to this embodiment includes the steps of: obtaining an X-ray spectrum obtained by irradiating a sample S with an electron beam EB and spectrally analyzing the X-rays emitted from the sample S using a WDS50a (an example of a first spectrometer); obtaining information on the time evolution of the intensity of correction element X-rays obtained by irradiating a sample S with an electron beam EB and spectrally analyzing the X-rays emitted from the sample S using a WDS50b (an example of a second spectrometer) and detecting the X-rays of correction element X-rays; and correcting the intensity of the X-rays of the target element in the X-ray spectrum based on the information on the time evolution of the intensity of correction element X-rays. Furthermore, in the step of correcting the intensity of the X-rays of the target element, information on the intensity of correction element X-rays detected at the same time as the X-rays of the target element is obtained from the information on the time evolution of the intensity of correction element X-rays, and the intensity of the X-rays of the target element is corrected based on the information on the intensity of correction element X-rays detected at the same time as the X-rays of the target element.

[0114] Therefore, in the analysis method according to this embodiment, the intensity of the X-rays of the element to be analyzed is corrected based on the intensity information of the X-rays of the correction element detected at the same time as the X-rays of the element to be analyzed, thus enabling accurate correction of the X-ray intensity of the element to be analyzed.

[0115] For example, when correcting the X-ray intensity of the element to be analyzed using information on the time change in the X-ray intensity of a correction element measured in advance, the X-ray intensity of the correction element may not change as measured in advance during the actual measurement. In contrast, the analysis method according to this embodiment can correct the X-ray intensity of the element to be analyzed based on information on the X-ray intensity of the correction element detected at the same time as the X-ray of the element to be analyzed, thus enabling accurate correction of the X-ray intensity of the element to be analyzed.

[0116] In the analysis method according to this embodiment, WDS50a has a spectroscopic element 52a (an example of a first spectroscopic element) that spectrally analyzes X-rays, and WDS50b has a spectroscopic element 52b (an example of a second spectroscopic element) that spectrally analyzes X-rays. Furthermore, in the step of acquiring the X-ray spectrum, the spectroscopic element 52a is moved in WDS50a and the X-ray spectrum is obtained by detecting X-rays of a wavelength corresponding to the position of the spectroscopic element 52a. Furthermore, in the step of acquiring information on the time change in the intensity of X-rays of the correction element, the position of the spectroscopic element 52b is fixed in WDS50b and information on the time change in the intensity of X-rays of the correction element is obtained by detecting X-rays of the correction element.Therefore, in the analysis method according to this embodiment, the X-ray spectrum and the time change in the intensity of X-rays of the correction element can be measured simultaneously.

[0117] In the analytical method according to this embodiment, the correction element is carbon. Furthermore, in the step of correcting the intensity of the X-rays of the correction element, the attenuation of the X-ray intensity of the analyte element caused by carbon is corrected based on information on the time change in the intensity of carbon's X-rays. Therefore, the analytical method according to this embodiment can correct for the effects of contamination mainly composed of carbon.

[0118] In the analytical method according to this embodiment, the correction element is an alkali metal contained in the sample S. Furthermore, in the step of correcting the X-ray intensity of the element to be analyzed, the time of the X-ray intensity of the correction element is measured. Based on the information about the changes, the concentration of the correction element is determined, and the concentration of the analyte is corrected based on the concentration of the correction element. Therefore, the analytical method according to this embodiment can accurately analyze the composition of a sample containing alkali metals.

[0119] In the analytical instrument 100, the processing unit 60 performs the following processes: acquiring an X-ray spectrum obtained by spectrally analyzing the X-rays emitted from the sample S using WDS50a; acquiring information on the time evolution of the intensity of the correction element's X-rays obtained by spectrally analyzing the X-rays emitted from the sample S using WDS50b and detecting the X-rays of the correction element; and correcting the intensity of the X-rays of the target element based on the information on the time evolution of the correction element's X-ray intensity. Furthermore, in the process of correcting the intensity of the X-rays of the target element, information on the intensity of the correction element's X-rays detected at the same time as the X-rays of the target element is obtained from the information on the time evolution of the correction element's X-ray intensity, and the intensity of the X-rays of the target element is corrected based on the information on the intensity of the correction element's X-rays detected at the same time as the X-rays of the target element.

[0120] Therefore, in the analytical device 100, the processing unit 60 corrects the intensity of the X-rays of the element to be analyzed based on the intensity information of the X-rays of the correction element detected at the same time as the X-rays of the element to be analyzed, thus enabling accurate correction of the X-ray intensity of the element to be analyzed.

[0121] In the analyzer 100, the processing unit 60, in the process of acquiring the X-ray spectrum, moves the spectroscopic element 52a of the WDS 50a and controls the WDS 50a so that X-rays of a wavelength corresponding to the position of the spectroscopic element 52a are detected, thereby acquiring the X-ray spectrum. Furthermore, in the process of acquiring information on the time change in the intensity of X-rays of the correction element, the processing unit 60 fixes the position of the spectroscopic element 52b of the WDS 50b and controls the WDS 50b so that X-rays of the correction element are detected, thereby acquiring information on the time change in the intensity of X-rays of the correction element. Therefore, the analyzer 100 can simultaneously measure the X-ray spectrum and the time change in the intensity of X-rays of the correction element.

[0122] In the analytical instrument 100, the correction element is carbon, and the processing unit 60, in the process of correcting the X-ray intensity of the element to be analyzed, corrects the attenuation of the X-ray intensity of the element to be analyzed due to carbon based on information on the time change in the X-ray intensity of the correction element. Therefore, the analytical instrument 100 can correct for the effects of contamination mainly composed of carbon.

[0123] In the analytical instrument 100, the correction element is an alkali metal contained in the sample S. In the processing unit 60, in the process of correcting the X-ray intensity of the element to be analyzed, the concentration of the correction element is determined based on information on the time change in the X-ray intensity of the correction element, and the concentration of the element to be analyzed is corrected based on the concentration of the correction element. Therefore, the analytical instrument 100 can accurately analyze the composition of a sample containing alkali metals that decrease due to electron beam irradiation.

[0124] 7. Variations It should be noted that the present invention is not limited to the embodiments described above, and various modifications can be implemented within the scope of the gist of the present invention.

[0125] For example, in the embodiment described above, the processing unit 60 corrected the spectrum using information on the time evolution of the spectrum and the X-ray intensity of the correction element measured using the analyzer 100. However, the processing unit 60 may also correct the spectrum using information on the time evolution of the spectrum and the X-ray intensity of the correction element obtained from another analyzer.

[0126] Furthermore, in the embodiment described above, as shown in Figure 5, in spectral imaging, a map analysis is performed to acquire map data by fixing the spectral position L, and this is repeated while changing the spectral position L to acquire multiple map data, and a spectral map SM is generated based on the acquired multiple map data. This is not limited to the above. For example, a spectral map may be generated by performing point analysis, in which the spectral position L is changed for each analysis point on the sample S and a spectrum is acquired. The spectral map acquired in this way can also be corrected in the same manner as in the embodiments described above.

[0127] The present invention is not limited to the embodiments described above, and various further modifications are possible. For example, the present invention includes configurations that are substantially identical to those described in the embodiments. A substantially identical configuration is, for example, a configuration that has the same function, method, and result, or a configuration that has the same purpose and effect. The present invention also includes configurations in which non-essential parts of the configuration described in the embodiments are replaced. Furthermore, the present invention includes configurations that produce the same effects or achieve the same purpose as the configuration described in the embodiments. Furthermore, the present invention includes configurations that add known technology to the configuration described in the embodiments. [Explanation of Symbols]

[0128] 10...Electron optics system, 12...Electron gun, 14...Focusing lens, 16...Decliner, 18...Objective lens, 20...Sample stage, 30...Electron detector, 52a...Spectrometer, 52b...Spectrometer, 54a...X-ray detector, 54b...X-ray detector, 60...Processing unit, 62...Control unit, 64...Calculation unit, 66...Display control unit, 70...Operation unit, 72...Display unit, 74...Storage unit, 100...Analyzer

Claims

1. An analytical method using an analytical apparatus equipped with multiple wavelength-dispersive X-ray spectrometers, A step of obtaining an X-ray spectrum obtained by irradiating a sample with an electron beam and spectrally analyzing the X-rays emitted from the sample using at least one first spectrometer among the plurality of wavelength-dispersive X-ray spectrometers, A step of obtaining information on the time change in the intensity of the X-rays of the correction element, obtained by irradiating the sample with an electron beam, spectrally analyzing the X-rays emitted from the sample using at least one second spectrometer among the plurality of wavelength-dispersive X-ray spectrometers, and detecting the X-rays of the correction element. A step of correcting the X-ray intensity of the element to be analyzed in the X-ray spectrum based on information on the time change of the X-ray intensity of the correction element, Includes, In the step of correcting the X-ray intensity of the element to be analyzed, From the time-dependent information on the intensity of the X-rays of the correction element, information on the intensity of the X-rays of the correction element detected at the same time as the X-rays of the element to be analyzed is obtained. An analytical method for correcting the intensity of X-rays of an element to be analyzed based on information about the intensity of X-rays of a correction element detected at the same time as the X-rays of the element to be analyzed.

2. In claim 1, The first spectrometer has a first spectroscopic element for spectrally separating X-rays, The second spectrometer has a second spectroscopic element for spectrally separating X-rays, In the step of acquiring the X-ray spectrum, the X-ray spectrum obtained by moving the first spectrometer and detecting X-rays of a wavelength corresponding to the position of the first spectrometer is acquired. The analysis method involves acquiring information on the time change in the intensity of the X-rays of the correction element in the step of acquiring information on the time change in the intensity of the X-rays of the correction element obtained by detecting the X-rays of the correction element in the second spectrometer with the position of the second spectroscopic element fixed.

3. In claim 1, The analytical method involves, in the step of acquiring the X-ray spectrum, acquiring a spectral map in which each position on the sample and the X-ray spectrum are associated and stored.

4. In claim 1, The aforementioned correction element is carbon, in this analytical method.

5. In claim 4, An analytical method comprising the step of correcting the X-ray intensity of the element to be analyzed, in which the attenuation of the X-ray intensity of the element to be analyzed due to carbon is corrected based on information on the time change of the X-ray intensity of the correction element.

6. In claim 1, The analytical method wherein the correction element is an alkali metal contained in the sample.

7. In claim 6, An analytical method comprising the step of correcting the X-ray intensity of the element to be analyzed, wherein the concentration of the correction element is determined based on information on the time change of the X-ray intensity of the correction element, and the concentration of the element to be analyzed is corrected based on the concentration of the correction element.

8. An electron optical system that irradiates a sample with an electron beam, Multiple wavelength-dispersive X-ray spectrometers for spectrally analyzing the X-rays emitted from the sample, A processing unit that corrects the intensity of X-rays of the element to be analyzed in the X-ray spectrum, Includes, The aforementioned processing unit, A process to obtain the X-ray spectrum obtained by spectrally analyzing the X-rays emitted from the sample using at least one first spectrometer among the plurality of wavelength-dispersive X-ray spectrometers, A process to obtain information on the time change in the intensity of the X-rays of the correction element, obtained by spectrally analyzing the X-rays emitted from the sample using at least one second spectrometer among the plurality of wavelength-dispersive X-ray spectrometers and detecting the X-rays of the correction element, A process to correct the X-ray intensity of the element to be analyzed based on information on the time change in the X-ray intensity of the correction element, Perform In the process of correcting the X-ray intensity of the element to be analyzed, From the time-varying information of the X-ray intensity of the correction element, information on the intensity of the X-ray of the correction element detected at the same timing as the X-ray of the element to be analyzed is obtained. An analytical apparatus that corrects the intensity of the X-rays of the element to be analyzed based on information about the intensity of the X-rays of the correction element detected at the same time as the X-rays of the element to be analyzed.

9. In claim 8, The first spectrometer has a first spectroscopic element for spectrally separating X-rays, The second spectrometer has a second spectroscopic element for spectrally separating X-rays, The processing unit, in the process of acquiring the X-ray spectrum, moves the first spectrometer and controls the first spectrometer so that X-rays of a wavelength corresponding to the position of the first spectrometer are detected, thereby acquiring the X-ray spectrum. The processing unit, in the process of acquiring information on the time change in the intensity of the X-rays of the correction element, fixes the position of the second spectrometer and controls the second spectrometer so that the X-rays of the correction element are detected, thereby acquiring information on the time change in the intensity of the X-rays of the correction element.

10. In claim 8, The processing unit is an analytical device that, in the process of acquiring the X-ray spectrum, acquires a spectral map in which each position on the sample and the X-ray spectrum are associated and stored.

11. In claim 8, The aforementioned correction element is carbon, in the analytical apparatus.

12. In claim 11, The processing unit is an analytical apparatus that, in a process of correcting the intensity of the X-rays of the element to be analyzed, corrects the attenuation of the X-ray intensity of the element to be analyzed caused by carbon, based on information on the time change in the intensity of the X-rays of the correction element.

13. In claim 8, The analytical apparatus wherein the correction element is an alkali metal contained in the sample.

14. In claim 13, The processing unit is an analytical apparatus that, in a process of correcting the X-ray intensity of the element to be analyzed, determines the concentration of the correction element based on information on the time change of the X-ray intensity of the correction element, and corrects the concentration of the element to be analyzed based on the concentration of the correction element.

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