JP2000121583A - Discrimination method for diameter of sample mask in x-ray fluorescence analysis and x-ray fluorescence analyzer - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide such a discrimination method for the diameter of a mask that can eliminate a measuring error in an X-ray analysis without requiring a special apparatus and increasing the number of elements to be measured, and that can discriminate the diameter of the mask in a short time. SOLUTION: A sample stage 19 which supports sample 1 is moved in the radial direction of a mask 3. In parallel with this operation, scattered rays by one kind or a plurality of kinds of fluorescent X-rays B2 which are generated from a part on the mask 3 or by primary X-rays B1 which are reflected by the mask 3 are detected through a diaphragm hole 14A for visual-field restriction. The intensity of the detected X-rays is compared with a reference intensity, and the diameter of a mask hole 4 is discriminated.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for judging the hole diameter (mask diameter) of a mask used for X-ray analysis of a sample, and an X-ray fluorescence analyzer for implementing the method.

[0002]

2. Description of the Related Art Generally, when performing X-ray analysis of a sample, a plurality of types of masks having different hole diameters are prepared, and a mask corresponding to the sample size is selected from these masks, and the sample is coated. Primary X-rays are irradiated to the measurement surface exposed from the mask hole of the sample, and the fluorescent X-rays generated from this measurement surface are detected by being squeezed with a field limiting aperture having a hole diameter corresponding to the mask hole diameter. I have. The above X-ray analysis is automatically performed by inputting various measurement conditions to the X-ray fluorescence spectrometer. At this time, one of the measurement conditions is a hole diameter of a mask selected according to a sample size. The aperture diameter corresponding to (mask diameter) is input to the X-ray fluorescence analyzer.

[0003] When selecting a mask diameter according to the sample size, conventionally, the mask diameter is determined by the following method. (1) Visual determination. (2) Discrimination by labels such as bar codes. (3) Discrimination using different materials corresponding to the mask diameter. (4) Discrimination using a slit.

[0004] In the visual discrimination (1), the mask diameter is visually confirmed or manually measured mechanically to determine the mask diameter. In the discrimination using a barcode in (2), for example, a barcode corresponding to a mask diameter is provided on a sample holder, and the barcode is read by a dedicated reader to determine the mask diameter (Japanese Patent Laid-Open No. 6-34).
No. 0443). Further, the discrimination using a different material corresponding to the mask diameter in (3) is based on the fact that at least the surface of the mask is treated with different kinds of specific elements (elements whose content in the sample is minute or zero) according to the size of the mask diameter. The mask diameter is determined by measuring the intensity of fluorescent X-rays from a specific element (JP-A-8-184573). In the discrimination using the slit in (4), at least the surface of the mask is formed of a material made of the above-described specific element, and the mask passes through the field limiting slit while changing the hole diameter of the field limiting slit through which the fluorescent X-ray passes. The mask diameter is determined by measuring the intensity of fluorescent X-rays from the specific element (Japanese Patent Application Laid-Open No. 8-184573). In this case, the same specific element can be used for a plurality of masks having different mask diameters.

[0005]

However, when the mask diameter is visually checked or measured manually, mistakes are likely to occur. Therefore, erroneous measurement conditions may be input to the X-ray fluorescence analyzer.

Further, when a bar code is provided on the sample holder and the mask diameter is determined using the bar code, only one mask can be attached to one holder. Therefore, many holders corresponding to each mask are required. In addition, a special device such as a reading device for reading the barcode is separately required. In addition, it is conceivable that a barcode is directly attached to the surface of each of the masks to determine the mask diameter. In this case, however, a barcode reading device is additionally required, and the X-ray analysis requires a separate barcode reader. Cannot be adopted because barcodes may be destroyed.

Further, when a different material corresponding to the mask diameter is used for the mask, there is a problem that the number of the measurement elements increases by the amount of the specific element, and the intensity of the fluorescent X-rays is changed while changing the hole diameter of the field limiting slit. However, it takes a long time to determine the mask diameter, and if the material of the mask is the same as that of the sample, the determination becomes impossible.

The present invention has been made in view of the above-described problems, and requires a special apparatus and does not increase the number of elements to be measured. An object of the present invention is to provide a method of determining a mask diameter that can eliminate measurement errors at the time of X-ray analysis, and a fluorescent X-ray analyzer using the same.

[0009]

In order to achieve the above object, a method of determining a sample mask diameter in X-ray analysis and an X-ray fluorescence analyzer for implementing the method according to the present invention cover a sample with a mask and mask holes. Exposes the measurement surface of the sample, irradiates the measurement surface with primary X-rays, and emits fluorescent X-rays generated from the sample.
During X-ray analysis for detecting a line and analyzing a sample, one or more fluorescent X-rays generated from a portion on the mask while moving a sample stage supporting the sample in the radial direction of the mask, or The scattered rays of the primary X-rays reflected by the mask are detected through the aperture for restricting the visual field, and the diameter of the mask aperture is determined by comparison with the reference intensity.

According to the present invention, the mask diameter can be determined by measuring the fluorescent X-rays generated from the mask and the scattered X-rays reflected by the mask, so that a special device is required. The determination of the mask diameter can be accurately performed in a short time without increasing the number of measurement elements, and measurement errors during X-ray analysis can be eliminated. In addition, this makes it possible to accurately select an aperture having a hole diameter corresponding to the mask diameter. Further, in the case of using scattered primary X-rays, the mask diameter can be determined irrespective of the material of the mask, so that the mask can be manufactured at low cost.

In a preferred embodiment of the discriminating method and apparatus according to the present invention, the measurement target area on the mask limited by the aperture is set smaller than the radial width of the thin portion on the inner diameter side of the mask.

According to the above-described method and apparatus, the scattered X-ray and primary X-ray from the thick portion of the mask and the scattered X-ray and primary X-ray from the thin portion of the mask are compared. Can be clearly distinguished, so that the mask diameter can be determined more accurately.

In a further preferred embodiment of the present invention, the slit member having an aperture for limiting the field of view of the fluorescent X-rays has an aperture having a plurality of apertures corresponding to a plurality of mask diameters. The plurality of mask diameters and the plurality of apertures are stored in the storage unit in association with the apertures, and the corresponding hole diameters read from the storage unit based on the mask diameter determined by the mask diameter determination method,
Alternatively, an aperture having a smaller diameter than this is arranged in the fluorescent X-ray extraction passage.

According to the above-described apparatus, the aperture corresponding to the determined mask diameter or the aperture having a smaller diameter than the determined mask diameter can be automatically arranged in the fluorescent X-ray extraction passage. The selection of the aperture can be performed correctly. Therefore, for example, when performing a qualitative analysis of the sample, there is no possibility that a fluorescent X-ray from the material portion of the mask is detected by passing through the aperture to cause a measurement error, and accurate measurement can be performed.

In a further preferred embodiment of the present invention, the slit member having an aperture for limiting the field of view of the fluorescent X-rays has an aperture having a plurality of apertures corresponding to a plurality of mask diameters. A desired hole diameter is set from among a plurality of hole diameters of the aperture of the slit member by an operation from the outside, and the slit member is driven so that the aperture of the set hole diameter is set in the fluorescent X-ray extraction passage. Arranged, the actual mask diameter determined by the mask diameter determination method,
When the diameter is smaller than the diameter of the arranged aperture, an error signal is output.

According to the above apparatus, for example, when quantitative analysis of a sample is performed, an aperture having a hole diameter set by an external operation as one of the measurement conditions is automatically arranged in a fluorescent X-ray extraction passage. When the determined actual mask diameter is smaller than the diameter of the corresponding aperture arranged, the fact can be confirmed by the output of the error signal, so that the fluorescent X-rays from the material portion of the mask can be confirmed. Accurate measurement can be performed without the risk of being detected through the aperture and causing a measurement error.

[0017]

Preferred embodiments of the present invention will be described below in detail with reference to the drawings. FIG. 1A shows a schematic configuration diagram of a fluorescent X-ray analyzer. In the figure, a sample 1 is held by a sample holder 2, a mask 3 having a hole diameter corresponding to the size of the sample 1 is selected and attached to the upper portion of the sample 1, and the mask 1 The measurement surface is exposed.

Further, the X-ray tube 5 irradiates the measurement surface of the sample 1 with primary X-rays B1 at an inclined angle, excites the sample 1 with the primary X-rays B1, and emits fluorescent X-rays specific to the element. Generate B2. This fluorescent X-ray B2 is incident on the spectroscope 6, and only the fluorescent X-ray B2 of a predetermined wavelength satisfying the Bragg equation is diffracted by the spectroscope 6, and the wavelength-dispersive fluorescent X-ray detector 7 is used.
Is detected by

As shown in FIGS. 2A and 2B, the mask 3 has a thick portion 3a on the outer diameter side and a thin portion 3b on the inner diameter side in order to determine the diameter of the mask hole 4. And a disc having an inclined portion 3c whose thickness gradually increases from the thin portion 3b toward the thick portion 3a, and a predetermined height difference d is set between the thick portion 3a and the thin portion 3b on the mask surface. I do. The mask 3
The inclined portion 3c is provided so that the step at the boundary between the thick portion 3a and the thin portion 3b does not become a shadow of the primary X-ray B1 from the X-ray tube 5 in the inclined posture.

The radial width of the thick portion 3a of the mask 3 is a, the radial width of the thin portion 3b is b, the radial width of the inclined portion 3c is c,
Assuming that the mask diameter (the diameter of the mask hole 4) is 2e, the radius m of the mask 3 is m = a + b + c + e. Further, between a plurality of masks 3 having different mask diameters 2e, respectively.
The radius m of the mask 3, the radial width c of the inclined portion 3c, and the radial width b of the thin portion 3b are constant. Therefore, as the mask diameter 2e increases (decreases), the radial width a of the thick portion 3a decreases (increases). The mask diameter 2e
Is, for example, 10 mmφ, 15 mmφ, 20 mmφ, 25 mm
Different ones such as φ and 30 mmφ are prepared in stages.

A disk-shaped slit member 10 is provided in the middle of the path of the fluorescent X-rays B2 reaching the spectroscope 6 shown in FIG. The slit member 10 has a rotation shaft 11 at the center. The pinion 12 meshing with a gear provided on the periphery of the slit member is driven by a motor 13 so that the slit member 10 rotates around the rotation shaft 11. In order to select a measurement target area on the mask 3 or the sample 2, for example, six circular aperture restricting holes 14 having different hole diameters are provided in the outer peripheral portion of the slit member 10 as shown in FIG. , 1
4A. The measurement target area is an area on the sample 1 or the mask 3 that can be seen from the detector 7 through the apertures 14 and 14A.

The motor 13 shown in FIG. 1A is connected to an aperture change circuit 15 for driving the motor to rotate the slit member 10 by a predetermined angle. The aperture driving circuit 35, the pinion 12, the motor 13, and the like constitute a slit driving unit 35. Further, the slit member 1
A mark 16 indicating the hole diameter number of the aperture hole 14, for example, a disk 16 in which a number of through holes or protrusions corresponding to the number are arranged on the circumference of the circle, is attached to the 0 rotation shaft 11. A sensor 17 for optically or magnetically detecting the mark is arranged facing the disk 16, and a hole diameter number detecting means 18 is connected to the sensor 17. With this configuration, the sensor 1
7, the hole diameter number detecting means 18 detects the hole diameter numbers corresponding to the apertures 14 and 14A located on the path of the fluorescent X-ray B2, and the detection output is transmitted to a control device 26 described later.
Is input to

The sample holder 2 includes a sample stage 19
The measurement position can be arbitrarily selected by moving the sample stage 19. The sample stage 19 is composed of an r-θ stage that moves in a rotational direction and a radial direction on a plane orthogonal to the axial direction of the cylindrical sample holder 2, and a motor 20 that performs θ drive and a linear moving device 21 that performs r drive Is driven by the moving means 22 composed of In this case, r
-θ is a polar coordinate with the center point of the sample surface at the time of sample measurement as a pole. The sample stage 19 moves in two directions orthogonal to each other on a plane orthogonal to the axial direction of the sample holder 2.
It may be a Y stage.

The X-ray fluorescence spectrometer has a control device 26 for controlling the whole apparatus in accordance with an inputted program. The control device 26 includes a mask diameter determining means 27, an aperture selecting means 36, and a memory 28. The detector 7
Is input to the signal processing circuit 29 and converted into an electric signal indicating the X-ray intensity. The output of the signal processing circuit 29 is input to the mask diameter determining means 27. The mask diameter determining means 27 determines the diameter of the mask hole 4 by comparing the X-ray intensity obtained from the signal processing circuit 29 with a reference intensity.

In the memory 28, the X-ray intensity when the thick portion 3a on the mask 3 is used as a measurement point is stored as a reference intensity. Separately, each mask 3 is stored in the memory 28.
The hole diameter of each mask 3 is stored in association with an intensity change detection distance at the time of mask diameter determination described later, and the hole diameter of each mask 3 is stored in association with a plurality of apertures 14 having a plurality of hole diameters corresponding to these hole diameters. .

The aperture selecting means 36 controls the slit driving means 35 at the time of discriminating the mask diameter or measuring the sample, and arranges the apertures 14 and 14A having a desired diameter in the extraction passage EP of the fluorescent X-ray B2. When the mask diameter is determined, the aperture 14A for determination is selected. Also, at the time of sample measurement, according to the mode set as the measurement conditions,
Two kinds of aperture selection operations are performed.

That is, when the automatic aperture selection mode is set as one of the measurement conditions, the corresponding aperture diameter read out from the memory 28 based on the mask diameter determined by the mask diameter determination means 27. Alternatively, the aperture hole 14 having a smaller hole diameter than the hole diameter corresponding to the mask diameter is selected. For example, when the diameter of the mask is 30 mm, the diameter of the corresponding aperture 14 is slightly smaller than the diameter of about 27 mm.
It is called an aperture diameter corresponding to a mask diameter of 0 mm. If there is no aperture 14 having a diameter corresponding to the determined mask diameter or smaller than the corresponding diameter, the aperture selecting means 3
The confirmation means 38 receiving the signal from 6 outputs an alarm signal notifying the fact. The confirmation means 38 outputs an alarm signal to, for example, a display (not shown) connected to the control device 26, displays a message or an image corresponding to the alarm signal on the screen thereof, and outputs the message or image via the control device 26. To stop the sample measurement operation.

When the hole diameter confirmation mode is set as one of the measurement conditions, the hole diameter selection means 36 selects the hole 14 having the hole diameter set by the operation of the hole diameter input means 37 from outside. . When the hole diameter confirmation mode is set, when the mask diameter determined by the mask diameter determination means 27 is smaller than the hole diameter of the aperture 14 set by the aperture diameter input means 37, the fact is notified. An error signal is output from the confirmation means 38. The error signal is also input to the display (not shown), a message or image corresponding to the error signal is displayed on the screen, and the sample measurement operation is stopped via the control device 36. The setting of the aperture diameter by the aperture diameter input means 37 is performed by inputting, for example, a number associated with the aperture diameter.

When determining the mask diameter, as described above,
Among the apertures 14 for restricting the visual field in the slit member 10, the smallest aperture 14A whose measurement target area is limited to a small diameter, for example, 1 mmφ, so that the thick portion 3a and the thin portion 3b of the mask 3 can be measured separately. Is selected. The diameter of the aperture 14A is such that the measurement target area on the mask 3 limited by the aperture 14A is smaller than the radial width b of the thin portion 3b, and X-rays from only the thin portion 3b are detected. The size is preferably as large as possible.

At the time of discriminating the mask diameter, the motor 13 is driven by a command given from the control device 26 to the aperture change circuit 15, and the slit member 10 rotates together with the disk 16. When the sensor 17 detects a mark corresponding to the aperture 14A among marks on the disk 16,
In response to the output of the hole diameter number detecting means 18 for detecting the hole diameter number based on the output of the sensor 17, the mask diameter determining means 27 gives a stop command to the aperture changing circuit 15. Thereby, the rotation of the slit member 10 is stopped, and the fluorescent X-ray B
The aperture 14A for discriminating the mask diameter is stopped on the second path. The other aperture 14 of the slit member 10 is used to limit the measurement target area on the sample surface when measuring the sample.

The linear moving machine 2 constituting the moving means 22
The first drive unit includes, for example, a stepping motor.
Connected to the linear moving device 21 is a moving distance detecting means 30 for detecting the moving distance of the sample stage 19 in the mask radial direction based on the number of pulses of the stepping motor. At the time of mask diameter determination, a detection signal of the moving distance detecting means 30 is input to the mask diameter determining means 27.

In the optical system including the X-ray tube 5 and the like, X-rays generated or reflected at the measurement point P (the center of the upper surface of the sample in FIG. 1A) and passing through the apertures 14 and 14A for restricting the visual field. As shown in FIG. 1 (B), the intensity becomes maximum at a height position H on the measurement surface of the sample, and decreases as the position shifts from the position H along a direction M perpendicular to the measurement surface. Characteristics are seen.

Focusing on such characteristics of the X-ray intensity distribution, mask diameter discrimination when X-ray analysis is performed by the fluorescent X-ray analyzer is performed as follows. That is, as described above, the aperture 1 for restricting the visual field in the slit member 10 is used.
In the state where the aperture 14A for discriminating the mask diameter is selected from the mask diameter discriminating holes 14A and 14A, the moving means 22 starts operating in response to a command from the mask diameter discriminating means 27, and as shown in FIG. The sample stage 19 moves in the radial direction of the mask 3 and stops until the measurement point P1 comes over the thick part 3a of the mask 3. The initial measurement point P1 is set so as to be on the thick portion 3a of any of the masks 3 having different mask diameters and to be at a constant width position (reference position) from the outer periphery of the mask toward the inner diameter side. You.

Next, the moving means 22 is driven in the opposite direction. As a result, as shown in FIG. 2A, the measurement point moves in the radial direction of the mask 3 at regular intervals (for example, 2.5 mm) from P1 to P2, P3,. A primary X-ray B2 partially scattered is detected through the aperture 14A in FIG. That is, the throttle hole 1
4A, the fluorescence X diffracted by the spectroscope 6 of FIG.
The intensity of the line B2 is detected by the detector 7, and the signal processing circuit 29
Is converted into an electric signal, and is input to the mask diameter determining means 27 of the control device 26. At the time of discriminating the mask diameter, the same primary X-ray B1 as that at the time of sample measurement is irradiated, and the primary X-ray B2 irrespective of the material is scattered from the mask 3.

The moving distance (2.5 mm) between the measurement points corresponds to the step diameter of the mask hole 4 changing stepwise at 5 mm intervals as described above. The measurement takes less time since it takes only a few places.

The mask diameter discriminating means 27 reads out the reference intensity from a memory 28 which stores the intensity of the fluorescent X-ray B2 when the thick portion 3a on the mask 3 is used as a measurement point, as a reference intensity. The coming X-ray intensity is compared with a reference intensity. When the measurement point is on the thick portion 3a of the mask 3, the X-ray intensity I input to the mask diameter determining means 27 is
The value is equal to the reference intensity. On the other hand, when the measurement point changes from above the thick portion 3a of the mask 3 to above the thin portion 3b, as shown in FIG. 4, the X-ray intensity input to the mask diameter determining means 27 becomes thicker. Difference d between the part 3a and the thin part 3b
And the value I + ΔI exceeding the reference intensity is obtained.

On the other hand, the mask diameter judging means 27 shown in FIG.
In parallel with the intensity comparison, the moving distance detecting means 30
The moving distance of the sample stage 19 detected by the measurement, that is, the moving distance of the measurement point is input. Then, as shown in FIG. 4, the mask diameter determining means 27 calculates the moving distance of the measurement point until the detected X-ray intensity changes to a value I + ΔI larger than the reference intensity, that is, the intensity change detection distance r. The mask diameter corresponding to the distance r is retrieved from the memory 28 to determine the mask diameter. That is, as shown in FIG. 2A, even if the mask diameter (the diameter of the mask hole 4) 2e is different, the radial widths b and c of the thin portion 3b and the inclined portion 3c and the radius m of the mask 3 are the same. Because of this, the radial width a of the thick portion 3a changes in proportion to the mask diameter 2e.
Since the intensity change detection distance r changes according to the radial width a of the thick portion 3a, it eventually corresponds to the mask hole 2e.
FIG. 5 shows the correspondence between the distance r stored in the memory 28 and the mask diameter 2e.

Accordingly, the mask diameter 2e is determined based on the correspondence between the distance r and the mask diameter 2e stored in the memory 28. The data of the determined mask diameter is saved in the control device 26 as one of the measurement conditions in the X-ray analysis of the sample 1.

In the mask diameter discrimination according to the above configuration, the mask diameter 2e is automatically and reliably determined in a short time by measuring the primary X-rays B2 scattered on the mask 3 irrespective of the material of the mask 3. The X-ray analysis of the sample 1 can be easily performed by inputting the measurement conditions according to the mask diameter 2e to the X-ray analyzer. Since the aperture 14 can be correctly selected according to the determined mask diameter, an erroneous measurement result due to an incorrect selection of the aperture 14 can be prevented.

Further, unlike the conventional example using a bar code, no special reading device is required.

Further, since it is not necessary to use a different material for each hole diameter of the mask 3, the mask 3 can be manufactured with the same material at low cost.

FIG. 6 is a flowchart showing an example of an operation of automatically determining a mask diameter and measuring a sample by the X-ray fluorescence analyzer. This operation is performed, for example, on sample 1
Is different from the case of the quantitative analysis described below, and the hole diameter (corresponding to the measurement area) of the aperture 14 of the slit member 10 does not need to be constant. First, in step S1, various measurement conditions necessary for controlling the apparatus at the time of qualitative analysis are input and set. Here, as one of the measurement conditions, an automatic aperture selection mode, which is one of the operation modes of the aperture selection means 36 at the time of measurement, is selectively set. In the next step S2, the operation of the apparatus is started, and in step S3, the above-described automatic determination of the mask diameter is performed.

Further, in the next step S4, it is confirmed whether or not the aperture member 14 having the hole diameter corresponding to the determined mask diameter exists in the slit member 10. The confirmation is performed by the aperture selection means 36 of the control device 26. That is, the aperture selection means 36 determines the memory 2 based on the determined mask diameter.
The stored data of No. 8 is searched to determine whether or not there is an aperture 14 having a hole diameter corresponding to the mask diameter. If there is a corresponding aperture 14, the aperture selector 36 controls the slit driver 35 to place the aperture 14 in the extraction path EP of the fluorescent X-ray B2 (step S5). With the aperture 14 selected in this way, the analysis of the sample 1 is started according to the measurement conditions set previously (step S).
6). In this case, since the actual mask diameter and the corresponding aperture 14 are selected, the fluorescent X-rays B2 from the material portion of the mask 3 pass through the aperture 14 and are detected by the detector 7. No measurement result containing incorrect information is obtained.

If it is determined in step S4 that there is no aperture hole 14 corresponding to the determined mask diameter,
The process shifts to step S7, where the aperture selecting means 3
6 is a throttle hole 14 having a smaller hole diameter than the corresponding hole diameter.
From the data stored in the memory 28. This allows
When the narrow hole 14 having a small hole diameter can be searched (step S
8) The process proceeds to step S5, where the aperture 14 is selected by the aperture selecting means 36, and further proceeds to step S6, where the analysis of the sample 1 is started. In this manner, even when there is no aperture hole 14 having a hole diameter corresponding to the actual mask diameter,
Since the aperture 14 having a smaller diameter than the corresponding aperture is selected, the fluorescent X-rays B2 from the material portion of the mask 3 are not detected through the aperture 14 and contain erroneous information. No measurement results are obtained. In this case, since the qualitative analysis of the sample 1 is performed, even if the aperture diameter of the aperture hole 14 is smaller than the aperture diameter corresponding to the mask diameter, it does not affect the suitability of the measurement result.

In step S8, if it is not possible to search for the aperture hole 14 having a smaller diameter than the determined mask diameter, the process proceeds to step S9, and the analysis of the sample 1 is stopped. In this case, an alarm signal notifying that there is no appropriate throttle hole 14 is output from the confirmation means 38.

FIG. 7 is a flowchart showing another example of the operation of automatically determining the mask diameter and measuring the sample by the X-ray fluorescence analyzer. This operation is, for example, for quantitative analysis of the sample 1. First, in step N1, various measurement conditions necessary for controlling the apparatus at the time of quantitative analysis are input and set. Here, as a part of the measurement conditions, a hole diameter confirmation mode, which is one of the operation modes of the aperture hole selection means 36 at the time of measurement, is selected and set, and an external input operation using the aperture diameter input means 37 is performed. In this case, a desirable hole diameter of the throttle hole 14 for quantitative analysis is set. As a result, the aperture selecting means 36 selects the aperture 14 having the input diameter, and the slit driving means 3
5 is arranged in the extraction passage EP of the fluorescent X-rays B2, and each part of the apparatus is adjusted according to other measurement conditions. In the next step N2, the operation of the apparatus is started, and in the next step N3, the above-described automatic determination of the mask diameter is performed in the same manner as in the flowchart of FIG.

Further, in the next step N4, the checking means 38 checks whether or not the determined mask diameter corresponds to the aperture diameter previously set as one of the measurement conditions. If the mask diameter corresponds to the set aperture diameter,
In the next step N5, quantitative analysis of the sample 1 is started according to the set measurement conditions. In this case, the actual mask diameter is set to the aperture hole 14 set and input as the measurement condition.
Therefore, the fluorescent X-ray B2 from the material portion of the mask 3 does not pass through the aperture 14 and is not detected, and a measurement result including incorrect information is not obtained.

If it is determined in step N4 that the determined mask diameter is different from the previously set corresponding aperture diameter, the process proceeds to step N6, where the determined mask diameter is set. It is confirmed whether the diameter of the corresponding aperture 14 is larger or smaller. If the determined mask diameter is larger, the process proceeds to the previous step N5,
The quantitative analysis of the sample 1 is started. In this case, the aperture 14
Since the diameter of the mask is larger than the hole diameter, the fluorescent X-rays B2 from the material portion of the mask 3 do not pass through the aperture 14 and are not detected, and a measurement result including incorrect information is not obtained.

If it is determined in step N6 that the determined mask diameter is smaller than the set diameter of the corresponding aperture 14, the process proceeds to step N7, where the quantitative analysis of the sample 1 is stopped. Is output. In this case, if the quantitative analysis is continued as it is, the fluorescent X-rays B1 from the material portion of the mask 3 will pass through the aperture hole 14 and an erroneous measurement result will be obtained. Can know that the mask diameter is not appropriate, and can reset the mask 3 having the appropriate mask diameter.

In FIG. 7, one of the measurement conditions is as follows.
Although the case where the hole diameter confirmation mode is selectively input and set has been described, when the hole diameter of the aperture hole 14 is input, the hole diameter confirmation mode is automatically selected, and the determined mask diameter is set to the set aperture diameter. Confirmation as to whether or not to respond may be performed automatically.

FIG. 7 shows a case where the hole diameter of the throttle hole 14 and the confirmation of the hole diameter selection mode are manually input as a part of the measurement conditions in the quantitative analysis. However, the same applies to the case of the qualitative analysis. The qualitative analysis may be performed by manually inputting the hole diameter of the throttle hole 14 and the confirmation of the hole diameter selection mode as a part of the measurement conditions.

In the above-described embodiment, the mask diameter is determined based on the intensity of the primary X-ray B2 scattered on the mask 3. However, the mask diameter is determined based on the fluorescent X-ray generated from the mask 3. Is also good. In this case, the mask diameter can be correctly determined by monitoring the X-ray specific to the material of the mask.

In addition, since the material of the mask 3 is different from the material used normally, the change in the intensity of the fluorescent X-rays from the mask cannot be sufficiently detected. Secondary X-rays of multiple elements (eg, FeKα
Line and rhodium scattered line) to detect a change in at least one of the two.

Further, an energy dispersive semiconductor detector (SSD) may be used as the detector 7 for detecting the intensity of the fluorescent X-rays or the scattered rays B2 of the primary X-rays. Be omitted.

[0055]

As described above, according to the present invention,
While moving the sample stage supporting the sample in the radial direction of the mask, one or more kinds of secondary X-rays generated from a part on the mask or primary X-rays reflected by the mask
Since the scattered radiation is detected through the aperture for restricting the visual field and the mask diameter is determined by comparing it with the reference intensity, a special device is required regardless of the material of the mask and the material of the sample, or special equipment or measurement is required. The mask diameter can be accurately determined in a short time without increasing the number of elements. In addition, since an aperture with a hole diameter suitable for the mask diameter can be correctly selected, measurement errors during X-ray analysis can be eliminated. Further, the mask can be manufactured at low cost.

[Brief description of the drawings]

FIG. 1A is a schematic configuration diagram showing an X-ray analyzer using a method of determining a sample mask diameter according to an embodiment of the present invention,
(B) is a diagram showing the distribution of X-ray intensity in the vertical direction at the center position of the measurement surface of the apparatus.

2A is a plan view of a mask, and FIG. 2B is a cross-sectional view of the same mask.

FIG. 3 is a front view of a slit member in the device.

FIG. 4 is a diagram showing a relationship between a change in X-ray intensity and a moving distance of a measurement point when a mask diameter is determined.

FIG. 5 is a diagram showing an example of contents stored in a memory.

FIG. 6 is a flowchart showing an example of an automatic analysis operation by the X-ray analyzer.

FIG. 7 is a flowchart showing another example of the automatic analysis operation by the apparatus.

[Explanation of symbols]

1 ... sample, 3 ... mask, 3a ... thick part, 3b ... thin part,
4 mask hole, 7 fluorescent X-ray detector, 10 slit member, 14A aperture hole, 19 sample stage, 22 moving means, 27 mask size discriminating means, 28 memory (storage means), 30 ... Moving distance detecting means, 35: slit driving means, 36: aperture selecting means, 37: aperture diameter inputting means,
38: confirmation means, EP: take-out passage

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Claims (6)

[Claims] 1. A sample is covered with a mask, a measurement surface of the sample is exposed by a mask hole, primary X-rays are irradiated on the measurement surface, and fluorescent X-rays generated from the sample are detected to analyze the sample. A method of determining a mask diameter in X-ray fluorescence analysis, wherein one or more fluorescent X-rays generated from a part on a mask while moving a sample stage supporting a sample in a radial direction of the mask, or Primary X reflected by mask
A method of determining a sample mask diameter in X-ray fluorescence analysis in which scattered X-rays are detected through an aperture for restricting a visual field and the diameter of the mask hole is determined by comparison with a reference intensity. 2. The sample mask diameter in X-ray fluorescence analysis according to claim 1, wherein an area to be measured on the mask limited by the aperture is set smaller than a radial width of a thin portion on the inner diameter side of the mask. Judgment method. 3. A fluorescent X-ray analyzer for irradiating a sample with primary X-rays and measuring fluorescent X-rays generated from the sample in a state where the sample is covered with a mask and a measurement surface of the sample is exposed by a mask hole. Moving means for moving the sample stage supporting the sample in the radial direction of the mask; a slit member having an aperture for restricting the field of view of the fluorescent X-rays; and one or more kinds generated from a part of the mask Fluorescence X
A detector for detecting the X-rays or primary X-ray scattered rays reflected by the mask through the aperture, and a mask diameter discrimination for discriminating the diameter of the mask hole by comparing the detected X-ray intensity with a reference intensity. X-ray fluorescence analyzer comprising: 4. The X-ray fluorescence spectrometer according to claim 3, wherein a measurement target area on the mask limited by the aperture is set smaller than a radial width of a thin portion on an inner diameter side of the mask. 5. The diaphragm according to claim 3, wherein the slit member has a plurality of apertures corresponding to a plurality of mask diameters, and the plurality of apertures has a plurality of apertures corresponding to a plurality of mask diameters. A slit driving unit that drives the slit member to arrange any one of the apertures in the fluorescent X-ray extraction passage; and a mask diameter determined by the mask diameter determining unit. Aperture means for driving the slit member such that a corresponding aperture read from the storage means or an aperture having a smaller diameter than the aperture is disposed in the fluorescent X-ray extraction passage. X-ray fluorescence analyzer. 6. The slit member according to claim 3, wherein the slit member has a plurality of apertures corresponding to a plurality of mask diameters, and a plurality of apertures of the slit member are externally operated. Aperture-diameter input means for setting a desired aperture from among the aperture diameters described above; slit drive means for driving the slit member to dispose an aperture having the set aperture diameter in a fluorescent X-ray extraction passage; and the mask A fluorescent X-ray analyzer comprising: a confirmation unit that outputs an error signal when the actual mask diameter determined by the diameter determination unit is smaller than the mask diameter corresponding to the diameter of the aperture hole arranged in the extraction passage.