Detection method and detection apparatus

Abstract

To provide a detection method and a detection device capable of increasing position resolution in a case of detecting characteristic values distributed within a plane of a sample s.SOLUTION: The present invention relates to a detection method for scanning an analysis range and detecting characteristic values distributed within a plane of a sample s. The detection method comprises: detecting the characteristic values of the sample s multiple times while moving the analysis range within the plane of the sample s so that some areas of the analysis range overlap; and performing statistical processing on detection results that include the same area and calculating characteristic values distributed within the plane of the sample s in units of overlapped areas.SELECTED DRAWING: Figure 1

Description

Technical Field

[0001] The present disclosure relates to a detection method for scanning an analysis range to detect characteristic values distributed in the plane of a sample, and a detection device.

Background Art

[0002] As an example of an apparatus for elemental analysis, a fluorescence X-ray analyzer is known. In a fluorescence X-ray analyzer, elemental analysis of a sample is performed by detecting fluorescence X-rays that reach a detector among the fluorescence X-rays generated from the range irradiated with primary X-rays. Therefore, in a fluorescence X-ray analyzer, the generation range of the fluorescence X-rays that reach the detector within the range irradiated with the primary X-rays becomes the analysis range, and average information on the amount of elements within the analysis range can be obtained.

[0003] In a fluorescence X-ray analyzer, when detecting the in-plane distribution of the amount of elements contained in a sample, it is necessary to change the range of the primary X-rays irradiated on the sample using a capillary and scan the analysis range of the sample in the plane of the sample. Specifically, International Publication No. 2020 / 084890 (Patent Document 1) discloses an X-ray analyzer that changes the range of primary X-rays irradiated using a capillary.

Prior Art Documents

Patent Documents

[0004]

Patent Document 1

Summary of the Invention

Problems to be Solved by the Invention

[0005] However, the positional resolution of the in-plane distribution of elemental amounts in a sample is determined by the relationship between the range of primary X-rays irradiating the sample and the range of fluorescent X-rays that reach the detector. Therefore, to improve positional resolution, it is necessary to either narrow the range of primary X-rays irradiating the sample or to make the detector itself smaller. Narrowing the range of primary X-rays irradiated required the use of a special capillary. Furthermore, narrowing the range of primary X-rays irradiated reduced the amount of X-rays that could be detected by the detector, leading to the problem of longer detection times.

[0006] This disclosure is made to solve the aforementioned problem and aims to provide a detection method and a detection apparatus that can improve the positional resolution when detecting characteristic values ​​distributed within the plane of a sample. [Means for solving the problem]

[0007] The detection method disclosed herein is a detection method that scans an analysis range to detect characteristic values ​​distributed within the plane of a sample. The detection method includes the steps of: detecting characteristic values ​​of a sample multiple times while moving the analysis range within the plane of the sample so that parts of the analysis range overlap; performing statistical processing on the detection results that include the same region and calculating characteristic values ​​distributed within the plane of the sample in units of overlapping regions; The steps include setting the number of regions to which the analysis range is divided as information on the positional resolution, Includes.

[0008] The detection device disclosed herein is a detection device for detecting characteristic values ​​distributed within the plane of a sample. The detection device comprises a detector for detecting characteristic values, a moving mechanism for scanning the analysis range of the sample, a control unit for controlling the detector and the moving mechanism, and a calculation unit for calculating characteristic values ​​distributed within the plane of the sample from the detection results detected by the detector. The control unit detects the characteristic values ​​of the sample multiple times with the detector while moving the analysis range within the plane of the sample so that a portion of the analysis range overlaps. The number of regions into which the analysis range is divided is set as information about the positional resolution. The calculation unit performs statistical processing on the detection results that include the same region and calculates characteristic values ​​distributed within the plane of the sample in units of overlapping regions. [Effects of the Invention]

[0009] The detection method and detection apparatus disclosed herein detect the characteristic values ​​of a sample multiple times while moving the analysis range within the plane of the sample so that a portion of the analysis range overlaps, thereby increasing the positional resolution when detecting characteristic values ​​distributed within the plane of the sample. [Brief explanation of the drawing]

[0010] [Figure 1] This is a schematic diagram of a detection device according to an embodiment. [Figure 2] This is a schematic diagram of another detection device according to the embodiment. [Figure 3] This is a schematic diagram illustrating the analytical range of the sample. [Figure 4] This is a flowchart showing a detection method according to an embodiment. [Figure 5] This is a schematic diagram showing the detection results obtained by the detection method according to the embodiment. [Figure 6] This is a schematic diagram illustrating the statistical processing of the detection method according to the embodiment. [Figure 7] This is a schematic diagram illustrating another statistical processing step of the detection method according to the embodiment. [Figure 8] This is a schematic diagram illustrating the scanning direction of the analysis range of the sample. [Modes for carrying out the invention]

[0011] The embodiments will be described in detail below with reference to the drawings. Note that the same or corresponding parts in the drawings are denoted by the same reference numerals, and their descriptions will not be repeated.

[0012] [Detection device] In this embodiment, a detection device for detecting characteristic values ​​distributed within the plane of a sample will be described below, with a fluorescent X-ray analyzer as an example. Of course, the detection device is not limited to a fluorescent X-ray analyzer, but any device capable of detecting characteristic values ​​distributed within the plane of a sample may be used. Examples include X-ray devices such as X-ray diffractometers (XRD), X-ray fluorescence film thickness gauges (XRF), X-ray microscopes (XRM), X-ray electron spectroscopy analyzers (XPS), ultraviolet photoelectron spectroscopy analyzers (UPS), and X-ray absorption fine structure analyzers (XAFS); spectroscopic devices such as spectrophotometers (terahertz, infrared, near-infrared, ultraviolet-visible), spectrofluorometers (RF), and solid-state emission spectrometers (OES); and microscopes such as fluorescence microscopes (MFM), scanning electron microscopes (SEM), transmission electron microscopes (TEM), and electron probe microanalyzers (EPMA).

[0013] In an X-ray fluorescence analyzer, the elements contained in a sample are analyzed by detecting the X-ray fluorescence that reaches the detector from the range of X-ray fluorescence generated from the area where the sample is irradiated with primary X-rays. Therefore, the characteristic value detected by the detector in an X-ray fluorescence analyzer may be not only the amount of X-ray fluorescence directly detected by the detector, but also the amount of elements calculated based on the detected amount of X-ray fluorescence. Furthermore, the characteristic value detected by the detector varies depending on the type of detection device; for a spectrometer, it is the intensity of the spectrally separated light or the physical property value based on the intensity of that light, and for an electron microscope, it is the reflected or transmitted electrons.

[0014] Figure 1 is a schematic diagram of a detection device according to an embodiment. The detection device 100 comprises a device body 10 and a signal processing device 20. The detection device 100 is an energy-dispersive X-ray fluorescence analyzer that analyzes the elements contained in a sample by observing the X-ray fluorescence emitted from the sample s to be analyzed.

[0015] First, the apparatus main body 10 will be described. The apparatus main body 10 includes an analysis chamber 110 in which a sample s is disposed, and an apparatus housing 120 in which an X-ray source 11, a collimator 12, and a detector 13 are disposed. The analysis chamber 110 has a plate-shaped sample base 111 and a cylindrical upper chamber 112 having a plate-shaped upper surface. In the central portion of the sample base 111, a circular opening 113 having a diameter of, for example, 15 mm is formed. The upper chamber 112 is attached to the sample base 111 so as to be openable and closable by an analyst or the like. In this specification, the plane on which the sample s is disposed is defined as the XY plane, and the direction orthogonal to the XY plane is defined as the Z-axis direction.

[0016] The X-ray source 11 is a point-focus X-ray tube, and for example, has a housing in which a target serving as an anode and a filament serving as a cathode are disposed. The X-ray source 11 is fixed to the apparatus housing 120 so that the X-ray emitted from the X-ray source 11 enters a predetermined irradiation range of the opening 113. Therefore, by placing the sample s on the sample base 111 so as to close the opening 113, the sample s within the predetermined irradiation range can be irradiated with X-rays.

[0017] As shown in FIG. 1, the collimator 12 is disposed between the X-ray source 11 and the opening 113, and is movable within a plane orthogonal to the optical axis of the X-ray by a moving device 14. By moving the collimator 12 with the moving device 14, the range of the X-ray irradiation within the plane of the sample s can be moved.

[0018] The detector 13 has, for example, a housing in which an introduction window is formed, and a detection element (semiconductor element) for detecting fluorescent X-rays is disposed inside the housing. The detector 13 is fixed so as to be located at the lower right of the opening 113 of the sample base 111, and is configured such that the fluorescent X-rays generated by the sample s enter the introduction window.

[0019] The detector 13 can identify the amount (intensity) of elements based on the intensity of the detected fluorescent X-rays. The detection device 100 can scan the analysis range obtained from the detection results detected by the detector 13 within the plane of the sample s by moving the area irradiated with X-rays using the collimator 12, and can detect the in-plane distribution of elemental amounts contained in the sample s. In the detection device 100, the area irradiated with X-rays corresponds to the analysis range of the sample s, as will be explained below, but it is also possible to irradiate the entire surface of the sample s with X-rays and scan the analysis range of the sample s by moving the detectable range of the detector 13.

[0020] Next, the signal processing device 20 will be described. The detection signal corresponding to the fluorescent X-ray detected by the main unit 10 is transmitted to the signal processing device 20. The signal processing device 20 includes a controller 22, a display 24, and an operation unit 26. The signal processing device 20 controls the operation of the main unit 10. The signal processing device 20 also analyzes the detection signal transmitted from the main unit 10 and displays the results based on the analysis on the display 24 or stores them in the memory 32.

[0021] The controller 22 has, as its main components, a processor 31, memory 32, a communication interface (I / F) 34, and an input / output I / F 36. Each of these components is connected to each other via a bus so that they can communicate with one another.

[0022] The processor 31 is typically an arithmetic processing unit such as a CPU (Central Processing Unit) or MPU (Micro Processing Unit). The processor 31 controls the operation of each part of the detection device 100 by reading and executing a program stored in the memory 32. Specifically, by executing the program, the processor 31 performs processing such as the analysis of fluorescent X-ray data based on the fluorescent X-rays detected by the detector 13. Although the example in Figure 1 illustrates a configuration with a single processor, the controller 22 may be configured to have multiple processors.

[0023] Memory 32 is implemented using non-volatile memory such as RAM (Random Access Memory), ROM (Read Only Memory), and flash memory. Memory 32 stores programs executed by the processor 31, or data used by the processor 31.

[0024] The input / output interface 36 is an interface for exchanging various types of data between the processor 31 and the display 24 and the operation unit 26.

[0025] The communication interface 34 is a communication interface for exchanging various signals and data with the main unit 10 of the device, and is implemented by an adapter or connector. The signal processing device 20 is connected to the X-ray source 11, the detector 13, and the mobile device 14 via the communication interface 34. The communication method may be a wired communication method or a wireless communication method such as a wireless LAN (Local Area Network).

[0026] A display 24 and an operation unit 26 are connected to the controller 22. The display 24 consists of an image-displaying liquid crystal panel or the like. The operation unit 26 receives user input for the detection device 100. The operation unit 26 typically consists of a touch panel, keyboard, mouse, or the like.

[0027] In the detection device 100, the analysis range can be moved within the plane of the sample s by moving the area to which X-rays are irradiated within the plane of the sample s. However, the means of moving the area to which X-rays are irradiated within the plane of the sample s can be achieved not only by moving the collimator 12 with the moving device 14 as described in Figure 1, but also by moving the sample s itself. Figure 2 is a schematic diagram of another detection device 100a according to the embodiment. In the detection device 100a shown in Figure 2, the same reference numerals are used for components that are the same as those in the detection device 100 shown in Figure 1, and detailed explanations are omitted.

[0028] The detection device 100a shown in Figure 2 has a sample holder 15 on which the sample s is placed, and the sample holder 15 can be moved in the XY plane of the sample base 111 by a moving device 14a. Therefore, in the detection device 100a, by moving the sample holder 15 with the moving device 14a, the portion of the sample s that covers the opening 113 can be moved, and the range of X-ray irradiation within the plane of the sample s can be moved. In the detection device 100a, the analysis range is moved within the plane of the sample s by moving the sample s itself.

[0029] [Detection method] Figure 3 is a schematic diagram illustrating the analysis range of sample s. Figure 3(a) shows how the amount of a certain element changes within the plane in sample s. Specifically, in range Xa, the amount of the element is "90", which is higher than in other ranges. Furthermore, it is assumed that the amount of the element changes within the plane in units divided into 12 × 12 regions (S(1,1) to S(12,12)) as shown in Figure 3(a). Therefore, if the analysis range of sample s is approximately the same as one of the regions divided into 12 × 12 regions, the detection device 100 can accurately detect the in-plane distribution of the amount of elements contained in sample s.

[0030] However, the area within the plane of the sample s that is irradiated with X-rays is divided into four regions, each a 12 × 12 grid, as shown in Figure 3(a). In other words, the detector 13 has four regions as one analysis range. Therefore, the detection device 100 scans the analysis range of the sample s in units of four regions, from region S(1,1) to region S(12,12), to detect the in-plane distribution of elemental amounts contained in the sample s.

[0031] Figure 3(b) shows the results of detecting the in-plane distribution of elemental amounts contained in sample s by scanning the analysis range of sample s in four regional units. The detection result for range A shown in Figure 3(b) is the average value of the elemental amounts in the four regions contained within range A shown in the corresponding Figure 3(a). Similarly, the detection results for ranges B and C shown in Figure 3(b) are the average values ​​of the elemental amounts in the four regions contained within ranges B and C, respectively, shown in the corresponding Figure 3(a). In other words, the detection device 100 can detect the in-plane distribution of elemental amounts contained in sample s in units divided into 6 × 6 regions (P(1,1) to P(6,6)) as shown in Figure 3(b).

[0032] The detection device 100 can only obtain detection results in units divided into a 6x6 area as shown in Figure 3(b), resulting in low spatial resolution for detecting the in-plane distribution of elemental amounts contained in the sample s, and thus it is not possible to accurately detect the in-plane distribution of elemental amounts. In particular, in the area Xa shown in Figure 3(a), the area where the elemental amount was "90" has decreased to "26" in the detection result shown in Figure 3(b), and the area with a higher elemental amount compared to other areas has expanded.

[0033] Therefore, in the detection device 100 according to this embodiment, instead of simply scanning the analysis range of the sample s in units of four regions, the elemental amounts of the sample s are detected multiple times while moving the analysis range within the plane of the sample s so that some regions of the analysis ranges overlap. Figure 4 is a flowchart of the detection method according to the embodiment. Figure 5 is a schematic diagram showing the detection results detected by the detection method according to the embodiment.

[0034] First, the controller 22 determines whether or not it has received positional resolution information (step S101). Here, the number of regions into which the analysis range will be divided is set as positional resolution information. If the controller 22 has received positional resolution information input by the user from the operation unit 26 (YES in step S101), it divides the analysis range into nx regions in the X direction and ny regions in the Y direction based on the input positional resolution information (step S102). Specifically, if the user provides, for example, positional resolution information of 1 / 4 of the analysis range, the controller 22 divides the analysis range into 4 regions, nx=2 in the X direction and ny=2 in the Y direction, as shown in Figure 5. If the controller 22 has not received positional resolution information (NO in step S101), it returns to step S101 and waits for the user to input positional resolution information from the operation unit 26. Of course, if the controller 22 has not received positional resolution information (NO in step S101), it may also select predetermined positional resolution information (for example, 1 / 4 of the analysis range).

[0035] If the input positional resolution information is 1 / 4 of the analysis range, the controller 22 calculates the elemental amount for each of the four regions by dividing the analysis range of sample s into two in the X direction and two in the Y direction, as shown in Figure 5, by setting nx=2 and ny=2. If the input positional resolution information is 1 / 9 of the analysis range, the controller 22 calculates the elemental amount for each of the nine regions by dividing the analysis range of sample s into three in the X direction and three in the Y direction, by setting nx=3 and ny=3. Furthermore, if the input positional resolution information is 1 / 3 of the analysis range, the controller 22 calculates the elemental amount for each of the two regions by dividing the analysis range of sample s into one in the X direction and two in the Y direction, by setting nx=1 and ny=2.

[0036] Next, the controller 22 scans the analysis range of the sample s so that some areas of the analysis range (for example, at least one of the divided areas) overlap (step S103). Specifically, the controller 22 controls the moving devices 14, 14a to move the collimator 12 or the sample holder 15, thereby moving the area to which X-rays are irradiated within the plane of the sample s, and thus scanning the analysis range of the sample s in units of overlapping areas (for example, one of the divided areas).

[0037] As shown in Figure 5(a), when focusing on region S(1,1), the analysis range of sample s is scanned so that it overlaps four times with the following regions: region W which includes region S(1,1) to the lower right, region X which includes region S(1,1) to the lower left, region Y which includes region S(1,1) to the upper left, and region Z which includes region S(1,1) to the upper right. The analysis range of sample s is scanned similarly for the other regions S, until the analysis range of sample s is scanned up to region S(12,12). Note that, as shown in Figure 5(a), it is assumed that sample s exists outside the detection target by at least one region.

[0038] The controller 22 acquires the detection result of the detector 13 each time it scans the analysis range of the sample s (step S104). Specifically, since the elemental amount in each region included in range W is "5", the detection result for range W is "5". Similarly, since the elemental amount in each region included in range X is "5", the detection result for range X is "5", since the elemental amount in each region included in range Y is "5", the detection result for range Y is "5", and since the elemental amount in each region included in range Z is "5", the detection result for range Z is "5". Note that the detector 13 can only acquire average information on the elemental amounts within the analysis range, and cannot actually know the elemental amounts of individual regions.

[0039] The controller 22 performs a statistical process to calculate the average value for detection results that include the same region, and calculates the elemental amount in units of overlapping regions (step S105). Specifically, when the controller 22 focuses on region S(1,1), it calculates the detection result P(1,1) corresponding to region S(1,1) by averaging the detection results "5" for range W, range X, range Y, and range Z (Equation 1). P(1,1)=(W+X+Y+Z) / 4=(5+5+5+5) / 4=5 (Formula 1) Similarly, when focusing on region S(7,3), the detection result for range R is "5" because the elemental amount in each region included in range R is "5", and the detection result for range T is "5" because the elemental amount in each region included in range T is "5". The detection result for range U is approximately "26" because there are three elements with an elemental amount of "5" and one element with an elemental amount of "90" in each region included in range U. The detection result for range V is "5" because there is an elemental amount of "5" in each region included in range V. In this embodiment, elemental amounts are expressed as integers by rounding to the nearest integer. The controller 22 calculates the detection result P(7,3) corresponding to region S(7,3) by averaging the detection results "5" for range R, "5" for range T, "26" for range U, and "5" for range V (Equation 2). P(7,3) = (R + T + U + V) / 4 =(5+5+26+5) / 4=approx. 10 (Formula 2) Similarly, when focusing on region S(8,4), the detection result for region U is approximately "26" because each region within that region contains three elements of "5" and one element of "90". The detection result for region K is "48" because each region within that region contains two elements of "5" and two elements of "90". The detection result for region O is "90" because each region within that region contains "90". The detection result for region Q is "48" because each region within that region contains two elements of "5" and two elements of "90". The controller 22 calculates the detection result P(8,4) corresponding to region S(8,4) by averaging the detection results for region U ("26"), region K ("48"), region O ("90"), and region R ("48") (Equation 3). P(8,4) = (U + K + O + Q) / 4 =(26+48+90+48) / 4=approx. 53 (Formula 3) The detection device 100, by performing the detection method shown in Figure 4, shows a higher elemental amount of "53" compared to the detection result shown in Figure 3(b), as shown in Figure 5(b). Furthermore, the detection device 100 obtains detection results in units divided into 12 × 12 areas, as shown in Figure 5(b), and can detect the in-plane distribution of elemental amounts contained in the sample s with high spatial resolution, enabling accurate detection of the in-plane distribution of elemental amounts. Moreover, by performing the detection method shown in Figure 4, the detection device 100 achieves a spatial resolution four times greater in the detection result shown in Figure 5(b) compared to the detection result shown in Figure 3(b).

[0040] [Statistical processing] Figure 5(b) illustrates that the controller 22 calculates the average value for detection results containing the same region and calculates the elemental amount in units of overlapping regions. However, the statistical processing performed on detection results containing the same region is not limited to calculating the average value; other statistical processing methods such as calculating the median or mode may also be used.

[0041] Figure 6 is a schematic diagram illustrating the statistical processing of the detection method according to the embodiment. Figure 6(a) shows how the amount of a certain element changes within the plane in sample s. Specifically, the amount of an element changes within the plane in units divided into 16 × 16 regions (S(1,1) to S(16,16)). In particular, the amount of an element is "90" in regions S(9,6), S(9,7), S(10,6), and S(10,7), which is higher than in other ranges.

[0042] For the sample s shown in Figure 6(a), the detection device 100 performs the detection method shown in Figure 4 to calculate the average value for detection results that include the same region, and the results of calculating the elemental amount in units of overlapping regions are shown in Figure 6(b).

[0043] In Figure 6(a), when focusing on region S(8,6), the elemental amount in each region included in range E is "5", so the detection result for range E is "5". In range F, there are three elements with an elemental amount of "5" and one element with an elemental amount of "90", so the detection result for range F is approximately "26". In range G, there are two elements with an elemental amount of "5" and two elements with an elemental amount of "90", so the detection result for range G is approximately "48". In range H, there is an elemental amount of "5", so the detection result for range H is "5". The controller 22 calculates the detection result P(8,6) corresponding to region S(8,6) by averaging the detection results of range E ("5"), range F ("26"), range G ("48"), and range H ("5") (Equation 4). P(8,6) = (E + F + G + H) / 4 =(5+26+48+5) / 4=21 (Formula 4) Similarly, when focusing on region S(9,6), the elemental amounts in each region within region F are 3 "5" and 1 "90", so the detection result for region F is approximately "26". The elemental amounts in each region within region G are 2 "5" and 2 "90", so the detection result for region G is "48". The elemental amounts in each region within region I are 2 "5" and 2 "90", so the detection result for region I is "48". The elemental amount in each region within region J is "90", so the detection result for region J is "90". Controller 22 calculates the detection result P(9,6) corresponding to region S(9,6) by averaging the detection results for region F (26), region G (48), region I (48), and region J (90) (Equation 5). P(9,6)=(F+G+I+J) / 4 =(26+48+48+90) / 4=approximately 53 (Formula 5) Next, Figure 7 is a schematic diagram illustrating another statistical processing of the detection method according to the embodiment. In Figure 7(a), the controller 22 calculates the median for the detection results containing the same region for the sample s shown in Figure 6(a), and calculates the elemental amount in units of the overlapping region. Specifically, in Figure 6(a), when focusing on region S(8,6), the controller 22 calculates the median from the detection results "5" in range E, "26" in range F, "48" in range G, and "5" in range H, and calculates the detection result M(8,6) corresponding to region S(8,6) (Equation 6). M(8,6) = MEDIAN(E,F,G,H) =MEDIAN(5,26,48,5)=16 (Formula 6) Similarly, when focusing on region S(9,6), the controller 22 calculates the median from the detection results of range F ("26"), range G ("48"), range I ("48"), and range J ("90") to determine the detection result M(9,6) corresponding to region S(9,6) (Equation 7). M(9,6)=MEDIAN(F,G,I,J) =MEDIAN(26,48,48,90)=48 (Formula 7) The detection device 100 calculates the median rather than the mean as a statistical process, resulting in a smaller maximum value of "48" in the detection results shown in Figure 7(a) compared to the detection results shown in Figure 6(b). However, the range of high elemental amounts in the detection results shown in Figure 7(a) is narrower compared to the detection results shown in Figure 6(b).

[0044] Next, in Figure 7(b), the controller 22 calculates the mode for the detection results containing the same region for the sample s shown in Figure 6(a), and calculates the elemental amount in units of the overlapping region. Specifically, in Figure 6(a), when focusing on region S(8,6), the controller 22 calculates the mode from the detection results "5" in range E, "26" in range F, "48" in range G, and "5" in range H, and calculates the detection result N(8,6) corresponding to region S(8,6) (Equation 8). N(8,6)=MODE(E,F,G,H) =MODE(5,26,48,5)=5 (Formula 8) Similarly, when focusing on region S(9,6), the controller 22 calculates the mode from the detection results of range F ("26"), range G ("48"), range I ("48"), and range J ("90") and calculates the detection result N(9,6) corresponding to region S(9,6) (Equation 9). N(9,6)=MODE(F,G,I,J) =MODE(26,48,48,90)=48 (Formula 9) The detection device 100 calculates the mode rather than the mean as a statistical process, resulting in a smaller maximum value of "48" in the detection results shown in Figure 7(b) compared to the detection results shown in Figure 6(b). However, the range of high elemental amounts in the detection results shown in Figure 7(b) is narrower compared to the detection results shown in Figures 6(b) and 7(a). In the detection results shown in Figure 7(b), the range of high elemental amounts coincides with the sample s shown in Figure 6(a), indicating high spatial resolution.

[0045] [Scanning direction] Figure 5(b) explains that the controller 22 obtains four detection results for the same region, calculates the average value of the four detection results, and calculates the elemental amount in units of overlapping regions. However, for example, if we want to know more about the in-plane distribution of the elemental amount of a sample in one direction, we can divide the analysis range of the sample s to increase the positional resolution in the direction we want to know more about, while not dividing the analysis range of the sample s in other directions, thereby reducing the number of detection results required.

[0046] Figure 8 is a schematic diagram illustrating the scanning direction of the sample analysis range. In Figure 8(a), the elemental amounts are calculated using the detection method shown in Figure 4, after dividing the analysis range of sample s shown in Figure 6(a) in the X direction (left-right direction in the figure). In other words, this is the case when the number of divisions of the analysis range of sample s (nx=2, ny=1) is accepted in step S101 shown in Figure 4. In Figure 8(a), the in-plane distribution of elemental amounts contained in sample s is detected in units divided into a 16×8 range (P(1,1)~P(16,8)).

[0047] Specifically, in Figure 6(a), when focusing on regions S(9,5) and S(9,6), the controller 22 calculates the detection result P1(9,3) corresponding to regions S(9,5) and S(9,6) by averaging the detection result "26" for range F and the detection result "48" for range I (Equation 10). P1(9,3)=(F+I) / 2=(26+48) / 2=37 (Equation 10) On the other hand, Figure 8(b) shows the results of calculating the elemental amounts using the detection method shown in Figure 4, after dividing the analysis range of the sample s shown in Figure 6(a) in the Y direction (up and down direction in the figure). In other words, this is the case when the number of divisions of the analysis range of the sample s (nx=1,ny=2) is accepted in step S101 shown in Figure 4. In Figure 8(b), the in-plane distribution of elemental amounts contained in the sample s is detected in units divided into an 8×16 range (P(1,1) to P(8,16)).

[0048] Specifically, in Figure 6(a), when focusing on regions S(9,6) and S(10,6), the controller 22 calculates the detection result P2(5,6) corresponding to regions S(9,6) and S(10,6) by averaging the detection result "48" for range I and the detection result "90" for range J (Equation 11). P2(5,6)=(I+J) / 2=(48+90) / 2=69 (Equation 11) In the example shown in Figure 8, the number of divisions in the analysis range of sample s is reduced to two (nx=2, ny=1) or (nx=1, ny=2) to reduce the number of detection results obtained. However, the number of detection results obtained can also be reduced without reducing the number of divisions in the analysis range. Specifically, the number of divisions in the analysis range of sample s can remain at four (nx=2, ny=2), and the number of detection results obtained can be reduced by scanning the analysis range in the Y or X direction in units of two regions. In other words, when the analysis range of sample s is divided into n (a natural number greater than or equal to 2) regions, the detection device 100 detects the characteristic values ​​of sample s multiple times such that there are fewer than n detection results containing the same region.

[0049] [Aspect] Those skilled in the art will understand that the embodiments described above are specific examples of the following embodiments.

[0050] (Section 1) A detection method according to one embodiment is a detection method for scanning an analysis range to detect characteristic values ​​distributed within the plane of a sample, and includes the steps of: detecting characteristic values ​​of a sample multiple times while moving the analysis range within the plane of the sample so that parts of the analysis range overlap; and performing statistical processing on the detection results that include the same region, and calculating characteristic values ​​distributed within the plane of the sample in units of overlapping regions.

[0051] According to the detection method described in paragraph 1, the characteristic values ​​of the sample are detected multiple times while moving the analysis range of the sample within the plane of the sample so that parts of the analysis ranges overlap, and statistical processing is performed on the detection results that include the same region. This makes it possible to improve the positional resolution when detecting characteristic values ​​distributed within the plane of the sample.

[0052] (Section 2) The detection method described in paragraph 1, further comprising the step of setting the number of regions into which the analysis range is divided as information on the positional resolution.

[0053] According to the detection method described in Section 2, the number of regions into which the analysis range is divided can be set as information for the positional resolution, allowing the user to freely change the positional resolution of the analysis range.

[0054] (Section 3) The detection method described in paragraph 1 or 2, wherein the statistical processing is the process of determining one of the following values: the mean, the median, or the mode.

[0055] According to the detection method described in paragraph 3, an appropriate statistical process can be selected from among several options depending on the type of sample.

[0056] (Section 4) In the detection method described in any one of paragraphs 1 to 3, if a portion of the overlapping analysis range is defined as a region obtained by dividing the analysis range into n (2 or more natural numbers) regions, then statistical processing is performed on the n detection results that include the same region to calculate characteristic values.

[0057] According to the detection method described in Section 4, the positional resolution when detecting characteristic values ​​distributed within the plane of a sample can be increased by n times.

[0058] (Section 5) In the detection method described in any one of paragraphs 1 to 3, if a portion of the overlapping analysis range is defined as a region obtained by dividing the analysis range into n (a natural number of 2 or more) parts, the characteristic values ​​of the sample are detected multiple times such that there are fewer than n detection results containing the same region.

[0059] According to the detection method described in Section 5, the detection time can be shortened compared to the case where the characteristic values ​​of the sample are detected multiple times so that n detection results include the same region.

[0060] (Section 6) A detection device according to one embodiment is a detection device for detecting characteristic values ​​distributed within the plane of a sample, comprising: a detector for detecting characteristic values; a moving mechanism for scanning the analysis range of the sample; a control unit for controlling the detector and the moving mechanism; and a calculation unit for calculating characteristic values ​​distributed within the plane of the sample from the detection results detected by the detector. The control unit detects the characteristic values ​​of the sample multiple times with the detector while moving the analysis range within the plane of the sample so that parts of the analysis range overlap, and the calculation unit performs statistical processing on the detection results that include the same area and calculates characteristic values ​​distributed within the plane of the sample in units of overlapping areas.

[0061] According to the detection device described in Section 6, the characteristic values ​​of the sample are detected multiple times while the analysis range is moved within the plane of the sample so that parts of the analysis ranges overlap, and statistical processing is performed on the detection results that include the same region. This makes it possible to improve the positional resolution when detecting characteristic values ​​distributed within the plane of the sample.

[0062] (Section 7) The detection device described in paragraph 6, wherein the control unit sets the number of regions into which the analysis range is divided as positional resolution information.

[0063] According to the detection device described in Section 7, the number of regions into which the analysis range is divided can be set as positional resolution information, allowing the user to freely change the positional resolution of the analysis range.

[0064] (Section 8) The detection device described in paragraph 8 is one of the following: an X-ray device, a spectrometer, or a microscope.

[0065] According to the detection device described in Section 8, the positional resolution can be improved when detecting characteristic values ​​distributed within the plane of a sample in various devices.

[0066] The embodiments disclosed herein should be considered in all respects to be illustrative and not restrictive. The scope of the present invention is indicated by the claims rather than by the description of the embodiments above, and all modifications within the meaning and scope equivalent to the claims are intended to be included. [Explanation of symbols]

[0067] 10 Main unit, 11 X-ray source, 12 collimator, 13 detector, 14, 14a transfer device, 15 sample holder, 20 signal processing device, 22 controller, 24 display, 26 control unit, 31 processor, 32 memory, 34 communication I / F, 36 input / output I / F, 100, 100a detection device, 110 analysis chamber, 111 sample base, 112 upper chamber, 113 opening, 120 device housing.

Claims

1. A detection method that scans an analysis range to detect characteristic values ​​distributed within the plane of a sample, The steps include: detecting the characteristic values ​​of the sample multiple times while moving the analysis range within the plane of the sample such that a portion of the analysis range overlaps; The steps include performing statistical processing on detection results that include the same region, and calculating characteristic values ​​distributed within the plane of the sample in units of overlapping regions, A detection method comprising the step of setting the number of regions into which the analysis range is divided as information on the positional resolution.

2. The detection method according to claim 1, wherein the statistical processing is a process of determining the value of the mean, median, or mode.

3. The detection method according to claim 1 or claim 2, wherein when a portion of the overlapping analysis range is defined as a region obtained by dividing the analysis range into n (2 or more natural numbers) regions, the statistical processing is performed on n detection results that include the same region to calculate characteristic values.

4. The detection method according to claim 1 or claim 2, wherein, when a portion of the overlapping analysis range is defined as a region obtained by dividing the analysis range into n (2 or more natural numbers) regions, the characteristic values ​​of the sample are detected multiple times such that there are fewer than n detection results containing the same region.

5. A detection method for scanning an analysis range to detect characteristic values ​​distributed within the plane of a sample, The steps include: detecting the characteristic values ​​of the sample multiple times while moving the analysis range within the plane of the sample such that a portion of the analysis range overlaps; The process includes the steps of performing statistical processing on detection results that include the same region, and calculating characteristic values ​​distributed within the plane of the sample in units of overlapping regions, A detection method in which, when a portion of the overlapping analysis range is divided into n (2 or more natural numbers) regions, statistical processing is performed on the n detection results containing the same region to calculate characteristic values.

6. A detection method for detecting characteristic values ​​distributed within the plane of a sample by scanning an analysis range, The steps include: detecting the characteristic values ​​of the sample multiple times while moving the analysis range within the plane of the sample such that a portion of the analysis range overlaps; The process includes the steps of performing statistical processing on detection results that include the same region, and calculating characteristic values ​​distributed within the plane of the sample in units of overlapping regions, A detection method in which, when a portion of the overlapping analysis range is divided into n (2 or more natural numbers) regions, the characteristic values ​​of the sample are detected multiple times such that there are fewer than n detection results containing the same region.

7. A detection device for detecting characteristic values ​​distributed within the plane of a sample, A detector that detects characteristic values, A moving mechanism for scanning the analysis range of the sample, A control unit that controls the detector and the moving mechanism, The system includes a calculation unit that calculates characteristic values ​​distributed within the plane of the sample from the detection results detected by the detector, The control unit, The characteristic values ​​of the sample are detected multiple times by the detector while the analysis range is moved within the plane of the sample such that a portion of the analysis range overlaps with it. The number of regions into which the analysis range is divided is set as information about the positional resolution. The aforementioned arithmetic unit, A detection device that performs statistical processing on detection results that include the same region and calculates characteristic values ​​distributed within the plane of the sample in units of overlapping regions.

8. The detection device according to claim 7, wherein the detection device is one of the following: an X-ray device, a spectrometer, and a microscope.

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