JP2905448B2 - Method and apparatus for setting position of sample stage in X-ray analysis - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to an X-ray analysis for irradiating a sample fixed on a sample stage with primary X-rays to detect secondary X-rays, particularly fluorescent X-rays, generated from the sample. The present invention relates to a method and an apparatus for setting the position of the sample stage.

[0002]

2. Description of the Related Art Conventionally, for example, in a total reflection type fluorescent X-ray analysis, as shown in FIG. 7, an X-ray generated from an X-ray tube 31 is made monochromatic by a monochromator 32 to form a primary X-ray 3.
The sample 1 fixed to the sample stage 34 has, for example, 0.0
A small incident angle θ of about 5 degrees (for ease of illustration and understanding,
X-rays 8z reflected from the sample 1 are made incident on the detector 5 while escaping to the right in the drawing so as not to make the totally reflected X-rays 8z incident on the detector 5. , Conduct an analysis. Here, for accurate analysis, the incident angle θ should be within a range larger than 0 degree and smaller than the critical angle of total reflection so that an appropriate S / N ratio (hereinafter, referred to as an S / N ratio) is obtained in the analysis. , “Appropriate angle”), and the total reflection on the surface 1 a of the sample 1 is directly below the detector 5 (the central axis Y of the detector 5 and the primary X-ray 3
Must occur at the point of intersection O) with the traveling direction. Therefore, the following method is used.

First, assuming that the surface 1a of the sample 1 and the surface 34a of the sample stage 34 are parallel to each other, the sample 1 is fixed to the sample stage 34 inclined at an appropriate angle near the primary X-ray 3, and The sample stage 34 is moved in the vertical direction (height direction), that is, in the direction of the center axis Y of the detector 5 so that the intensity of the fluorescent X-rays 38 incident on the sample stage 5 is maximized.
Adjust the height of the. Thus, the position where total reflection occurs on the sample surface 1a can be located immediately below the detector 5. Next, while adjusting the angle of the sample stage 34 so that the incident angle θ to the sample 1 is gradually increased, the fluorescence X
The intensity change of the line 38 is measured by the detector 5. X-ray fluorescence 38
When the intensity of the background rapidly increases, the intensity of the background also rapidly increases, and the incident angle θ at this time is the critical angle. Since the critical angle is known according to the main component of the sample 1, the adjustment angle of the sample stage 34 and the angle of incidence θ on the sample 1
You can see the relationship with Then, the angle of the sample table 34 is adjusted so that the incident angle θ becomes an appropriate angle, and the sample 1 is analyzed.

At the time of analysis, if such adjustment is made for each sample 1, it takes a very long time. Then, with the sample 1 thus adjusted placed thereon, the sample stage 34 is moved by a predetermined distance xc in the traveling direction of the primary X-ray 3, that is, rightward in FIG. (Indicated by the two-dot chain line). The displacement sensor 39 is located on the right side of the detector 5 by a distance xc, and its central axis YC is parallel to the central axis Y of the detector 5, and both central axes Y and YC are in the traveling direction of the primary X-ray 3. It is vertical. Then, a laser beam 40 is emitted from the displacement sensor 39, and the laser beam 41 reflected on the sample surface 1a is measured.
Measure the distance to This distance is stored in the analyzer or the like as the height of the sample stage 34 at which total reflection occurs immediately below the detector 5. The relationship between the adjustment angle of the sample stage 34 and the angle of incidence θ on the sample 1 is also stored in an analyzer or the like.

When a new sample 1 is analyzed,
First, the sample 1 is fixed to a sample stage 34 located below the displacement sensor 39, and the sample stage 34 is moved up and down (height direction), that is, the displacement sensor 39 while using the displacement sensor 39.
By moving the sample table 34 in the direction of the center axis YC, the height of the sample table 34 is adjusted so that the distance from the displacement sensor 39 to the sample surface 1a becomes the stored distance. with this,
First, the position where total reflection occurs on the surface 1 a of the new sample 1 can be set immediately below the displacement sensor 39. Next, while maintaining the height of the sample table 34, the distance xc
Just return to the left. Thus, the position where total reflection occurs can be located immediately below the detector 5. Further, the angle of the sample stage 34 is adjusted to a desired appropriate angle by utilizing the stored relationship between the adjustment angle of the sample stage 34 and the incident angle θ to the sample 1, and the sample 1 is analyzed. .

Even if the thickness of each sample 1 is different, the distance used as a reference for adjusting the height of the sample table 34 is not affected since it is the distance from the displacement sensor 39 to the sample surface 1a. . Also, the sample surface 1a is the surface 3 of the sample table 34.
In the case where the sample table 34 is inclined with respect to 4a, the sample table 34 on which the sample 1 is fixed is moved by a predetermined distance (for example, 10 mm) in the left-right direction of FIG. Then, the distance from the displacement sensor 39 to the sample surface 1a is measured using the displacement sensor 39.
Since the inclination of the sample surface 1a can be calculated from the measurement distance at the left and right positions and the movement distance in the left and right direction, the angle adjustment of the sample table 34 can be corrected accordingly.

[0007]

However, in the prior art, the adjustment of the height of the sample stage 34 under the displacement sensor 39 is performed on the order of several μm, whereas the leftward adjustment after the adjustment is performed. The moving distance xc to is on the order of several cm,
The adjusted height is not always maintained after the movement. Therefore, the position of the sample table 34 cannot be set sufficiently accurately, and the sample 1 cannot be analyzed sufficiently accurately.

The present invention has been made in view of the above-mentioned conventional problems, and does not complicate the structure of the apparatus in X-ray analysis.
It is an object of the present invention to provide a method and an apparatus for setting the position of a sample stage that enable accurate analysis.

[0009]

According to a first aspect of the present invention, there is provided a method for setting a position of a sample stage in an X-ray analysis, the method comprising: Irradiation of primary X-rays from a source and reflection X-rays reflected on the surface of the sample at a first and second distances from a predetermined reference point in the traveling direction of the primary X-rays, the height of the reflected X-rays from the predetermined reference line The intensity distribution in the vertical direction is measured. Next, from the first and second intensity distributions, a shift from the position of the sample table at which total reflection occurs on the sample surface immediately below the analytical detector is obtained, and the analysis is performed so as to eliminate the shift. Below the detector for use, the angle between the surface of the sample stage and the primary X-ray and the height of the sample stage from the reference line are adjusted.

According to the method of the first aspect, since the position (height and angle) of the sample stage is adjusted below the analytical detector, there is no need to move the sample stage over a large distance after the adjustment. In addition, since the reference for adjusting the position of the sample stage is the position (height and angle) at which total reflection occurs on the sample surface immediately below the analytical detector, there is no need to move the sample stage by a fixed amount after adjustment. Analysis can be performed as it is. Therefore, the position of the sample stage can be set accurately. Further, since the X-ray source used for the analysis is used as it is, no new light source for adjustment is required.

According to a second aspect of the present invention, there is provided an apparatus for setting the position of a sample stage in X-ray analysis, comprising: a sample stage on which a sample is fixed; an X-ray source used for analysis and irradiating the sample with primary X-rays; An angle adjuster that is provided below the analytical detector and adjusts the angle between the surface of the sample stage and the primary X-ray; and an angle adjuster that is also provided below the analytical detector and extends from a predetermined reference line of the sample stage. A height adjuster for adjusting the height of the sample, and the height of the reflected X-rays reflected from the sample surface at the first and second distances from the predetermined reference point in the traveling direction of the primary X-rays. First and second reflected X-ray detecting means for measuring the intensity distribution in the vertical direction, respectively. In addition, the measured first
And from the second intensity distribution, an angle adjuster and a height adjuster are obtained so as to obtain a shift from the position of the sample stage at which total reflection occurs on the sample surface immediately below the analytical detector, and to eliminate the shift. Control means for controlling the vessel. According to the device of the second aspect, the same operation and effect as those of the method of the first aspect are obtained.

According to a third aspect of the present invention, in a method for setting the position of a sample stage in X-ray analysis, a sample fixed on the sample stage is irradiated with primary X-rays from an X-ray source used for analysis, and is shifted from a predetermined reference point by one.
At first and second distances in the traveling direction of the next X-ray,
The through-holes of the first and second shielding plates provided at a height such that the total reflection X-rays directly below the sample surface immediately below the analytical detector pass at the maximum intensity were reflected on the sample surface. In order for the reflected X-rays to pass and the intensity detected by the reflected X-ray detector to be maximum, below the analytical detector,
The angle between the surface of the sample stage and the primary X-ray and the height of the sample stage from a predetermined reference line are adjusted.

According to the method of the third aspect, in addition to the effect of the method of the first aspect, the total reflection occurs on the surface of the sample immediately below the analytical detector at the adjusted position of the sample stage. Since the confirmation is made, the position setting of the sample stage becomes more accurate.

According to a fourth aspect of the present invention, there is provided an apparatus for setting a position of a sample stage in X-ray analysis, comprising: a sample stage on which a sample is fixed; an X-ray source used for analysis and irradiating the sample with primary X-rays; An angle adjuster that is provided below the analytical detector and adjusts the angle between the surface of the sample stage and the primary X-ray; and an angle adjuster that is also provided below the analytical detector and extends from a predetermined reference line of the sample stage. A height adjuster for adjusting the height of the sample, a reflected X-ray detector for detecting reflected X-rays reflected on the sample surface, and a primary X-ray detector from a predetermined reference point.
At the first and second distances in the direction of travel of the line, a through hole is provided at a height such that the total reflection X-rays directly below the sample surface immediately below the analytical detector pass at maximum intensity. First and second shielding plates. Further, the angle adjuster and the height adjuster are arranged so that the reflected X-rays pass through the passage holes of the first and second shielding plates and the intensity detected by the reflected X-ray detector is maximized. It has control means for controlling. According to the device of the fourth aspect, the same operation and effect as the method of the third aspect can be obtained.

According to a fifth aspect of the present invention, in a method for setting the position of a sample stage in X-ray analysis, first, a sample fixed on the sample stage is irradiated with primary X-rays from an X-ray source also used for analysis, and a predetermined reference point is set. At a first distance in the direction of travel of the primary X-ray from the sample, the height is set such that the total reflection X-ray directly below the sample surface immediately below the analytical detector passes at the maximum intensity. The reflected X-ray reflected on the sample surface passes through the passage hole of the shielding plate,
To maximize the intensity detected by the reflected X-ray detector,
The height of the sample stage from a predetermined reference line is adjusted below the analytical detector. Next, at a second distance from the reference point in the traveling direction of the primary X-ray,
The intensity distribution in the height direction from the reference line is measured, and from the intensity distribution, a deviation from the position of the sample table that causes the total reflection X-ray immediately below is obtained. Below the detector, the angle between the surface of the sample stage and the primary X-ray and the height of the sample stage from the reference line are adjusted.

According to the fifth aspect of the present invention, first, the position of the sample table is adjusted to be closer to the position of the sample table which generates the total reflection X-ray directly below, and then the position of the sample table which generates the total reflection X-ray directly below is adjusted. Since the adjustment is made so as to eliminate the deviation from the position, the position of the sample stage can be set with an accuracy similar to the method of the third aspect and in a shorter time than the method of the third aspect.

The apparatus for setting the position of a sample stage in X-ray analysis according to claim 6 includes a sample stage on which a sample is fixed, an X-ray source which is also used for analysis and irradiates the sample with primary X-rays, An angle adjuster that is provided below the analytical detector and adjusts the angle between the surface of the sample stage and the primary X-ray; and an angle adjuster that is also provided below the analytical detector and extends from a predetermined reference line of the sample stage. A height adjuster for adjusting the height of the sample, a reflected X-ray detector for detecting reflected X-rays reflected on the sample surface, and a primary X-ray detector from a predetermined reference point.
At a first distance in the traveling direction of the line, a first hole provided with a passage hole at a height such that total reflection X-rays immediately below the sample surface directly below the analytical detector pass through at maximum intensity. A shielding plate, and a second shielding plate that is movable in the height direction from the reference line at a second distance from the reference point in the traveling direction of the primary X-ray and has a through hole. I have.

Further, a height adjuster is controlled so that the reflected X-rays pass through the passage hole of the first shielding plate and the intensity detected by the reflected X-ray detector becomes maximum. A sample stage that generates the total reflection X-ray immediately below from the intensity distribution in the height direction from the reference line measured by the reflection X-ray detector and the second shielding plate for the reflected X-ray after the control. Is provided with control means for controlling the angle adjuster and the height adjuster so as to obtain a deviation from the position and to eliminate the deviation. According to the device of the sixth aspect, the same operation and effect as those of the method of the fifth aspect can be obtained.

The apparatus for setting the position of the sample stage in the X-ray analysis according to claim 7 is the first and second apparatus according to claim 2.
The reflected X-ray detecting means is movable in the height direction from the reference line at each of the first and second distances from the reference point in the traveling direction of the primary X-ray, and is provided with a passage hole. 1,
Each of the second shielding plates and a common reflection X-ray detector are configured.

According to the apparatus of claim 7, the operation and effect of the apparatus of claim 2 are provided, and one reflected X-ray detector is sufficient for two reflected X-ray detecting means, so that the entire apparatus is not complicated. .

The apparatus for setting the position of the sample stage in the X-ray analysis according to claim 8 is the same as the apparatus according to claim 2,
Are the first and second charge-coupled devices that measure the first and second intensity distributions, respectively.

According to the device of the eighth aspect, in addition to the operation and effect of the device of the second aspect, the reflected X-ray detecting means is a charged coupling element capable of detecting a position.
The number of moving parts is reduced, and it is not complicated.

[0023]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, a method for setting the position of a sample stage in X-ray analysis according to a first embodiment of the present invention will be described with reference to the drawings. First, an apparatus used in this method will be described. As shown in the perspective view of FIG. 1, the apparatus comprises a sample stage 2 on which a sample 1 is fixed, and an X-ray source 4 which is also used for analysis and irradiates the sample 1 with a band-shaped primary X-ray 3. It has. Although only the X-ray tube is illustrated as the X-ray source 4, a monochromator or a slit may be included. Also,
This apparatus is provided below the detector for analysis 5 and
And an angle adjuster 6 for adjusting the angle between the surface 2a of the sample and the primary X-ray 3, and also provided below the analytical detector 5, for adjusting the height of the sample table 2 from a predetermined reference line X. And a height adjuster 7. Here, the center line of the band-shaped primary X-ray 3 and its extension are defined as a predetermined reference line X. In addition,
The height of the sample stage 2 may be, for example, the height from the reference line X to the center of the surface 2a of the sample stage 2.

Further, the present apparatus is arranged such that a predetermined reference point O
At the first and second distances x1 and x2 in the traveling direction of the next X-ray 3 (the direction toward the upper right in FIG. 1), the first and second shielding plates 9 provided with the passage holes 9a and 11a, respectively. , 11 and a reflected X-ray detector 13. Here, the intersection of the central axis Y of the detector 5 and the reference line X of the primary X-ray 3 is defined as a predetermined reference point O, and the first and second shielding plates 9 and 1 are provided.
Reference numeral 1 denotes the first and second moving means 10 and 12 along the central axes Y1 and Y2, which are parallel to the central axis 5 of the analysis detector 5, respectively, in the height direction from the reference line X. It is movable. The heights of the first and second shielding plates 9 and 11 are, for example, from the reference line X to the respective passing holes 9a and 9a.
What is necessary is just to take the height to the center of 11a.

The first shielding plate 9 and the reflected X-ray detector 13 constitute first reflected X-ray detecting means, and the second shielding plate 1
1 and the reflected X-ray detector 13 constitute a second reflected X-ray detecting means, and the reflected X-rays 8 reflected on the sample surface 1a are set at the first and second distances x1 and x2, respectively. The intensity distribution in the height direction from X is measured. Further, the present apparatus uses the measured first and second intensity distributions from the position of the sample stage 2 where total reflection occurs on the sample surface 1a immediately below the analytical detector 5 for the measured sample 1. And a control unit 14 for controlling the angle adjuster 6 and the height adjuster 7 so as to obtain the deviation and to eliminate the deviation. In the present invention, “total reflection occurs”
Then, as explained in the conventional technology,
The incident angle θ to the sample 1 is not only in a range larger than 0 degree but smaller than a critical angle of total reflection, and is desirably an appropriate angle such that an S / N ratio becomes good in analysis. .

Using this apparatus, in the method of the first embodiment, for example, the surface parallel to the sample stage surface 2a with a predetermined thickness is determined based on the geometrical relationship of the optical system, preliminary experiments, and the like. The sample stage 2 is initially set at a position where total reflection occurs on the sample surface 1a immediately below the analytical detector 5 when the standard sample 1 having the sample 1a is used. An X-ray source 4 for fixing a new sample 1 on the sample stage 2 and also used for analysis.
From the reference point O in the traveling direction of the primary X-ray 3 with respect to the reflected X-ray 8 reflected from the sample surface 1a as shown below. At x2, the first and second intensity distributions in the height direction from the reference line X are measured. First, the first and second shielding plates 9 and 11
Both are located above the path of the reflected X-rays 8, and the reflected X-rays 8 reflected on the sample surface 1 a enter the reflected X-ray detector 13 as they are. Therefore, first, the first moving means 1
By 0, the first shielding plate 9 is moved downward along the center axis Y1. Then, the reflected X-ray 8 is shielded by the first shielding plate 9 and does not enter the reflected X-ray detector 13.

However, when the first shielding plate 9 is further lowered, as shown in FIG.
When the passing holes 9a of the shielding plate 9 are matched, the reflected X-rays 8 pass through the passing holes 9a and enter the reflected X-ray detector 13. Here, strictly speaking, the reflected X-rays 8 not only have a width in the horizontal direction and are band-shaped, but also slightly spread, that is, have a thickness in a direction (up-down direction) perpendicular to the reference line X. Therefore, the height of the first shielding plate 9 through which the reflected X-rays 8 can pass through the passage hole 9a also has a width, and the reflected X-ray detector 1
The intensity of the reflected X-ray 8 detected in 3 is also obtained as an intensity distribution in the height direction having a certain width. Therefore, in this intensity distribution, it is assumed that the passage hole 9a of the first shielding plate 9 exactly matches the path of the reflected X-ray 8 at the height of the first shielding plate 9 where the maximum intensity is obtained.

After the first intensity distribution is obtained for the reflected X-rays 8 as described above, the first moving means retreats the first shielding plate 9 above the path of the reflected X-rays 8. Then, the state is returned to the initial state, and the second moving means 12
Is moved downward along its central axis Y2 to obtain a second intensity distribution in the same manner. At this time, the first shielding plate 9 is not retracted, and the reflection X passing through the passage hole 9a is not retreated.
The second shielding plate 11 may be lowered with respect to the line 8.
In this case, as shown in FIG. 1, the passage hole 11a of the second shielding plate 11 is preferably an elongated hole extending in the horizontal direction. The reflected X-rays 8 having passed through the passage holes 9a of the first shielding plate 9 and having a reduced width are slightly displaced in the horizontal direction of the second shielding plate 11 so that the reflected X-rays 8 are not reflected. ,
This is to prevent the passage through the passage hole 11a of the second shielding plate 11 from being prevented.

For example, in the case of total reflection X-ray fluorescence analysis, extremely high precision is required for the position adjustment of the sample table 2, and it is practically impossible to determine the reference line X as a reference at the design stage of the apparatus. It is. Therefore, as described above, the center line of the band-shaped primary X-ray 3 and its extension are set as the reference line X, and the path of the primary X-ray 3 in a state where the sample 1 is not irradiated is measured for the apparatus. There is a need. Therefore, in the method of the first embodiment, the sample stage 2 is retracted in advance by the height adjusting means 7 in advance and the first and second intensity distributions of the reflected X-ray 8 are measured in the same manner. By measuring the first and second intensity distributions of the primary X-ray 3 in the procedure described above, the path is examined, and this is set as a reference line X. This measurement also requires extremely high accuracy, and slight temporal changes in the path of the primary X-ray 3 may cause a problem.
It is desirable to perform the measurement again about once a day or once a week. It should be noted that this measurement is shorter than the whole analysis and does not need to be performed for each sample 1, so that the whole analysis time is not affected.

As described above, when the first and second intensity distributions of the reflected X-ray 8 in the height direction from the reference line X are measured, the data is input to the control means 14 as an electric signal. These measurements and inputs can also be performed automatically by the control means 14. The control means 14 analyzes the standard sample 1 having a predetermined thickness and a surface 1a parallel to the sample table surface 2a in advance based on the geometrical relationship of the optical system, preliminary experiments, and the like. Detector 5
Total reflection X-ray 8z directly reflected by the sample surface 1a immediately below
The passages 9 of the first and second shielding plates 9 and 11
The heights of the first and second shielding plates 9 and 11 from the reference line X when a and 11a exactly match are input. The position of the sample stage 2 at this time, that is, the angle between the surface 2a of the sample stage 2 and the primary X-ray 3 and the position of the sample stage 2
Is also referred to as a standard position below.

Since the sample stage 2 is initially set at the standard position as described above, the path of the reflected X-rays 8 is directly below the total reflection X-rays 8.
z and the reference of the first and second shielding plates 9 and 11 when the first and second passage holes 9a and 11a exactly match the path of the reflected X-ray 8. The height from the line X should also correspond to the height of the previously input immediately below total reflection X-rays 8z. However, even if it is intended to be manufactured in the same shape, the thickness may be slightly different depending on the sample 1 due to a problem of processing accuracy or the like. is there. Therefore, the sample stage 2
Is initially set to a preferable standard position for the standard sample 1, but for a new sample 1, a position where total reflection actually occurs on the sample surface 1a immediately below the analytical detector 5 (hereinafter, each position is referred to as Such a position of the sample 1 is also referred to as an “ideal position”) in many cases.

Therefore, in the method of the first embodiment, the control means 14 determines the first and second intensity distributions of the input reflected X-rays 8 in the path of the reflected X-rays 8 based on the first and second intensity distributions. The heights of the first and second shielding plates 9 and 11 from the reference line X when the passing holes 9a and 11a accurately coincide with each other are obtained. By comparing the height with the height, the deviation from the ideal position of the sample stage 2 is calculated from the geometrical relationship, and the angle between the sample stage surface 2a and the primary X-ray 3 is calculated so as to eliminate the deviation. The height of the sample table 2 from the reference line X is adjusted. Thereby, the sample stage 2 is set at the ideal position.

According to the method of the first embodiment, since the position of the sample stage 2 is adjusted below the analytical detector 5, there is no need to move the sample stage 2 over a large distance after the adjustment.
The reference for adjusting the position of the sample table 2 is, for example, the sample surface 1.
It is not a position where a is in contact with the primary X-ray 3 in parallel.
Since this is an ideal position where total reflection occurs on the sample surface 2a immediately below the analysis detector 5, it is not necessary to move the sample table 2 by a fixed amount after adjustment, and the analysis can be performed as it is. Therefore, the position of the sample table 2 can be set accurately, and the sample 1 can be accurately analyzed. Further, since the X-ray source 4 used for the analysis is used as it is, a new light source for adjustment is not required, and two reflected X-ray detecting means necessary for knowing the path of the reflected X-ray 8 are required. Two reflected X-ray detectors 13 are sufficient. Therefore, the entire apparatus used does not become complicated.

Next, a method for setting the position of the sample stage in the X-ray analysis according to the second embodiment of the present invention will be described with reference to the drawings. First, an apparatus used in this method will be described. As shown in the perspective view of FIG.
The first shielding plate 15 can shield the left half and the right half in the direction of travel of the reflected X-rays 8, and the second shielding plate 16 can shield the right and the left half. , 11 are different from the apparatus used in the method of the first embodiment which can shield the reflected X-rays 8 over the entire width. In other respects, the apparatus is the same as the apparatus used in the method of the first embodiment, and thus the same parts are denoted by the same reference numerals and description thereof will be omitted.

In the method of the second embodiment using this apparatus, the method of measuring the first and second intensity distributions of the reflected X-ray 8 is different from the method of the first embodiment as described below. That is, first, the first and second shielding plates 15, 1
6 indicates that each of the passage holes 15a and 16a has a reflection X
It is at a height slightly above the passage of the line 8 (height as shown in the second shielding plate 16 in FIG. 2). In this state, the reflected X-rays 8 pass through the first and second shielding plates 15 and 16.
And is not incident on the reflection X-ray detector 13.
Here, when only the first shielding plate 15 is moved downward along an axis Y1 perpendicular to the reference line X and parallel to the central axis of the analysis detector 5, as shown in FIG. Passage No. 8
When the passing hole 15a of the shielding plate 15 is matched, the reflected X-ray 8 passes through the passing hole 15a and the left side of the second shielding plate 16 and enters the reflected X-ray detector 13. Therefore, as described in the method of the first embodiment, the first intensity distribution is obtained for the reflected X-ray 8.

Next, the first moving means 10 returns the first shielding plate 9 to a height at which the passage hole 15a is slightly higher than the path of the reflected X-ray 8, that is, the first state. This movement amount is very small because the passage holes 15a and 16a are actually small like pinholes, but this movement causes the reflected X-rays 8 to again cause the first and second shielding plates to move. The light is shielded by 15 and 16 and does not enter the reflected X-ray detector 13. Therefore, the second moving means 12
By moving the second shield plate 16 downward along an axis Y2 perpendicular to the reference line X and parallel to the central axis of the analysis detector 5, the second shield plate 16 is moved in the second direction similarly to the first intensity distribution. An intensity distribution is obtained. Note that the primary X
The path of the line 3 is also examined by measuring the first and second intensity distributions, and this is set as a reference line X.
Other procedures are the same as the method of the first embodiment. According to the method of the second embodiment, in addition to the same operation and effect as the method of the first embodiment, the first and second shielding plates 15,
Since only a small amount of movement is required, the intensity distribution can be measured more quickly and accurately.

Next, a method for setting the position of the sample stage in the X-ray analysis according to the third embodiment of the present invention will be described with reference to the drawings. First, an apparatus used in this method will be described. As shown in the perspective view of FIG.
First and second reflected X-ray detectors measure the first and second intensity distributions, respectively, of the first and second charged coupling elements 17,
18, the first charged coupling element 17 is movable in the height direction from the reference line X by the first moving means 10, but the reflected X-ray 8 is incident on the second charged coupling element 18. It differs from the apparatus used in the method of the first embodiment in that it is fixed at a predetermined height from the reference line X. In other respects, the apparatus is the same as the apparatus used in the method of the first embodiment, and thus the same parts are denoted by the same reference numerals and description thereof will be omitted. Note that “first” in the first moving means 10 means that it corresponds to the first charged coupling element 17, and does not mean “first” among a plurality of moving means.

In the method of the third embodiment using this apparatus, the method of measuring the first and second intensity distributions of the reflected X-ray 8 differs from the method of the first embodiment as described below. That is, as shown in FIG. 3, first, the first charged coupling element 17 is located above the path of the reflected X-rays 8, and the reflected X-rays 8 are fixed to a predetermined height. The light enters the coupling element 18. Since the positions of the charged coupling elements 17 and 18 can be detected, the second intensity distribution can be measured without being moved.

Next, the first shielding plate 9 is moved down by the first moving means 10 along the central axis Y1 to a predetermined height from the reference line X where the reflected X-rays 8 are incident. Move. Thereby, the first intensity distribution can be measured similarly to the second intensity distribution. In the method of the third embodiment, in measuring the first intensity distribution, the first charged coupling element 17 does not need to be gradually moved, but is immediately lowered to a predetermined height, and the first charged coupling element 17 is moved to the first height at that height. Can be measured. The path of the primary X-ray 3 is measured by measuring the first and second intensity distributions of the primary X-ray 3 in advance in the same manner, and this is set as a reference line X. Other procedures are the same as the method of the first embodiment. That is,
In the method of the first embodiment, the first and second passage holes 9a, 1 are formed in the path of the reflected X-ray 8 or the total reflection X-ray 8z immediately below.
The height equivalent to the height of the first and second shielding plates 9 and 11 from the reference line X when 1a exactly matches the third shielding plate 9 and 11 is the third height.
In the method according to the embodiment, in the intensity distribution measurement of the reflected X-ray 8 or the total reflection X-ray 8z immediately below, the height from the reference line X at the position where the highest intensity is detected by the first and second charged coupling elements 17 and 18 Become.

According to the method of the third embodiment, the sample table 2
Is adjusted below the detector 5 for analysis,
There is no need to move the sample stage 2 over a large distance after the adjustment. Further, since the reference for adjusting the position of the sample stage 2 is an ideal position where total reflection occurs on the sample surface 2a immediately below the analysis detector 5, there is no need to move the sample stage 2 by a fixed amount after adjustment, and Perform analysis. Therefore, the sample stage 2
Can be set accurately, and the sample 1 can be accurately analyzed.
In addition, since the X-ray source 4 used for analysis is used as it is,
A new light source for adjustment is not required, and in particular, according to the method of the third embodiment, two reflected X-ray detecting means necessary to know the path of the reflected X-ray 8 are capable of position detection. The charge-coupled elements 17, 18 and the second charge-coupled element 18 can remain fixed, so that the number of movable parts is reduced. Therefore, the entire apparatus used does not become complicated.

Next, a method for setting the position of the sample stage in the X-ray analysis according to the fourth embodiment of the present invention will be described with reference to the drawings. First, an apparatus used in this method will be described. As shown in the perspective view of FIG.
The first charged coupling element 19 can detect about the left half in the traveling direction of the reflected X-ray 8, and the second charged coupling element 20 can detect the rest, so that the first and second charged coupling elements 17 can be detected. ,
18 differs from the apparatus used in the method of the third embodiment, which can detect the reflected X-rays 8 over the entire width. Further, in this device, not only the second charged coupling element 20 but also the first charged coupling element 19 is fixed at a predetermined height from the reference line X where the reflected X-ray 8 is incident. However, this is different from the apparatus used in the method of the third embodiment. In other respects, the apparatus is the same as the apparatus used in the method of the third embodiment, so that the same parts are denoted by the same reference numerals and description thereof is omitted.

In the method of the fourth embodiment using this apparatus, the method of measuring the first and second intensity distributions of the reflected X-ray 8 differs from the method of the third embodiment as described below. That is, as shown in FIG. 4, from the beginning, the reflected X-rays 8 are applied to the first and second charged coupling elements 19 and 20 fixed at a predetermined height, respectively, with approximately half of the left and the rest being left. Incident. Since the position of each of the charged coupling elements 19 and 20 can be detected, the first and second intensity distributions can be measured at the same time without being moved. The path of the primary X-ray 3 is measured by measuring the first and second intensity distributions of the primary X-ray 3 in advance in the same manner, and this is set as a reference line X. Other procedures are the same as the method of the third embodiment. According to the method of the fourth embodiment, in addition to the same operation and effect as the method of the third embodiment, the reflected X-ray detecting means are the charge coupling elements 19 and 20 capable of detecting the position,
Since both may remain fixed, the number of movable parts is further reduced in the entire apparatus used, and the apparatus is not complicated. Further, the intensity distribution can be measured more quickly and accurately.

Next, a method of setting the position of the sample stage in the X-ray analysis according to the fifth embodiment of the present invention will be described with reference to the drawings. First, an apparatus used in this method will be described. As shown in the perspective view of FIG.
Except when setting the reference line X in advance, the first and second shielding plates 21 and 22 are moved at the first and second distances x1 and x2 from the reference point O in the traveling direction of the primary X-ray 3. ,
It differs from the apparatus used in the method of the first embodiment in that passing holes 21a and 22a are provided at a height such that the total reflection X-rays 8z directly below pass at the maximum intensity, and are kept fixed. Further, as will be described later, the control contents performed by the control unit 23 are also different. In other respects, the apparatus is the same as the apparatus used in the method of the first embodiment, and thus the same parts are denoted by the same reference numerals and description thereof will be omitted. The passage hole 22a of the second shielding plate 22 may be a simple round hole or a long hole extending in the horizontal direction.

In the method of the fifth embodiment using this apparatus, first, the first and second intensity distributions of the primary X-ray 3 are measured in advance in the same procedure as the method of the first embodiment. To check the path, and set this as a reference line X. This measurement may be performed, for example, about once a day or once a week, as described above. Then the first
And the passage holes 21a, 22a of the second shielding plates 21, 22
However, the first and second moving means 1 are located at such a height that the total reflection X-rays 8z directly below each pass at the maximum intensity.
According to 0 and 12, the first and second shielding plates 21 and 22 are moved.

Then, the sample stage 2 initially set to the standard position
Then, a new sample 1 is fixed, and primary X-rays 3 are irradiated from an X-ray source 4 used for analysis. Next, the reflected X-rays 8 reflected on the sample surface 1a are applied to the first and second passage holes 21a, 22a.
a, and the height of the sample stage 2 from the reference line X so that the intensity detected by the reflected X-ray detector 13 is maximized. Is adjusted by the control means 23 little by little by trial and error. As a result, the sample stage 2 is set to the ideal position, and it is confirmed that the setting has been made. As described above, in the method of the fifth embodiment, except for setting the reference line X in advance,
The first and second shielding plates 21 and 22 remain fixed at predetermined heights, respectively.

According to the method of the fifth embodiment, the sample table 2
Is adjusted below the detector 5 for analysis,
There is no need to move the sample stage 2 over a large distance after the adjustment. Further, since the reference for adjusting the position of the sample stage 2 is an ideal position where total reflection occurs on the sample surface 2a immediately below the analysis detector 5, there is no need to move the sample stage 2 by a fixed amount after adjustment, and Perform analysis. Furthermore, especially this fifth
According to the method of the embodiment, at the adjusted position of the sample table 2, the path of the reflected X-rays 8 matches the path of the total reflection X-rays 8 z directly below, that is, the sample surface immediately below the analytical detector 5. It is confirmed that total reflection occurs in 1a. Therefore, the position of the sample table 2 can be set more accurately, and the sample 1
Can be analyzed more accurately. Further, since the X-ray source 4 used for analysis is used as it is, a new light source for adjustment is not required, and only one reflection X-ray detector 13 is required. Therefore, again, the entire apparatus to be used is not complicated.

Next, a method for setting the position of the sample stage in the X-ray analysis according to the sixth embodiment of the present invention will be described with reference to the drawings. First, an apparatus used in this method will be described. As shown in the perspective view of FIG.
Except when setting the reference line X in advance, only the first shielding plate 21 has a maximum total reflection X-ray 8z directly below the reference point O at the first distance x1 from the reference point O in the traveling direction of the primary X-ray 3. It differs from the apparatus used in the method of the fifth embodiment in that a passage hole 21a is provided at a height such that it passes with a high strength and remains fixed. Further, as will be described later, the control performed by the control unit 24 is also different. In other respects, the apparatus is the same as the apparatus used in the method of the fifth embodiment, and the same parts are denoted by the same reference numerals and description thereof will be omitted. The passage hole 11a of the second shielding plate 11 is preferably a long hole extending in the horizontal direction.

In this method, first, the first and second intensity distributions of the primary X-ray 3 are measured in advance in the method of the sixth embodiment in the same procedure as in the method of the first embodiment. To check the path, and set this as a reference line X. Then, the passage hole 21a of the first shielding plate 21 is
The first shielding means 2 is moved by the first moving means 10 so that the total reflection X-rays 8z directly underneath reach the height so as to pass with the maximum intensity.
1 is moved. Further, the second moving means 12 is arranged so that the second shielding plate 11 is located above the path of the reflected X-rays 8.
To move.

Then, the sample stage 2 initially set to the standard position
Then, a new sample 1 is fixed, and primary X-rays 3 are irradiated from an X-ray source 4 used for analysis. Next, the sample X-ray 8 reflected by the sample surface 1a passes through the passage hole 21a of the first shielding plate 21, and the intensity of the sample detected by the reflection X-ray detector 13 is maximized. Only the height from the reference line X of 2 is adjusted by the control means 24 little by little by trial and error.
The first passage hole 21a is provided at a height such that the total reflection X-ray 8z immediately below passes at the maximum intensity, similarly to the apparatus used in the method of the fifth embodiment. 2 is adjusted closer to the ideal position. Further, the second moving means 12 moves the second shielding plate 11 downward along the center axis Y2 to advance the primary X-ray 3 from the reference point O in the same manner as in the first embodiment. At a second distance x2 in the direction, the second intensity distribution of the reflected X-ray 8 in the height direction from the reference line X is measured.

In the method of the sixth embodiment, the reflected X-rays 8 are adjusted by the adjustment so that the reflected X-rays 8 at the first distance x1 from the reference point O in the traveling direction of the primary X-rays 3 are directly below the total reflection X
It passes through the first passage hole 21a at the same height as the line 8z. Therefore, in the control means 24, the input reflection X
From the second intensity distribution of the line 8, the height of the second shielding plate 11 from the reference line X when the second passage hole 11a exactly matches the path of the reflected X-ray 8 is obtained. Is compared with the height of the total reflection X-ray 8z immediately below input in advance, the deviation from the ideal position of the sample table 2 is calculated from the geometric relationship, and the deviation is eliminated.
The angle between the sample stage surface 2a and the primary X-ray 3 and the height of the sample stage 2 from the reference line X are adjusted. Thereby, the sample stage 2 is set at the ideal position. Thus, in the method of the sixth embodiment, the first shielding plate 21 remains fixed at the predetermined height except when the reference line X is set in advance.

According to the method of the sixth embodiment, first, only the height of the sample table 2 is adjusted by trial and error so as to be closer to the ideal position, and then the deviation from the ideal position is obtained. The sample table surface 2a and the primary X
Since the adjustment including the angle formed with the line 3 is performed, the position of the sample table 2 can be set in a shorter time with accuracy according to the method of the fifth embodiment.

[0052]

As described above, according to the present invention,
Since the position (height and angle) of the sample stage is adjusted below the analytical detector, there is no need to move the sample stage over a large distance after the adjustment. In addition, since the reference for adjusting the position of the sample stage is the position (height and angle) at which total reflection occurs on the sample surface immediately below the analytical detector, there is no need to move the sample stage by a fixed amount after adjustment. Analysis can be performed as it is. Therefore, the position of the sample stage can be set accurately, and the sample can be accurately analyzed. Further, since the X-ray source used for the analysis is used as it is, no new light source for adjustment is required, and the structure of the apparatus is not complicated.

[Brief description of the drawings]

FIG. 1 is a perspective view showing an apparatus used for a method for setting a position of a sample stage in an X-ray analysis according to a first embodiment of the present invention.

FIG. 2 is a perspective view showing an apparatus used for a method of setting a position of a sample stage in X-ray analysis according to a second embodiment of the present invention.

FIG. 3 is a perspective view showing an apparatus used for a method of setting a position of a sample stage in X-ray analysis according to a third embodiment of the present invention.

FIG. 4 is a perspective view showing an apparatus used for a method of setting a position of a sample stage in X-ray analysis according to a fourth embodiment of the present invention.

FIG. 5 is a perspective view showing an apparatus used for a method for setting a position of a sample stage in X-ray analysis according to a fifth embodiment of the present invention.

FIG. 6 is a perspective view showing an apparatus used for a method of setting a position of a sample stage in X-ray analysis according to a sixth embodiment of the present invention.

FIG. 7 is a side view showing an apparatus used for a conventional method for setting the position of a sample stage in total reflection X-ray fluorescence analysis.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... sample, 1a ... sample surface, 2 ... sample table, 2a ... sample table surface, 3 ... primary X-ray, 4 ... X-ray source also used for analysis, 5
... Analytical detector, 6 ... Angle adjuster, 7 ... Height adjuster, 8
... Reflection X-ray, 8z ... Total reflection X-ray directly below, 9, 15, 21 ...
1st shielding plate, 9a, 15a, 21a ... passage hole of 1st shielding plate, 10 ... 1st moving means, 11, 16, 22 ... 2nd shielding plate, 11a, 16a, 22a ... 2nd Passing hole of shielding plate, 12: second moving means, 13: reflected X-ray detector, 14, 23, 24: control means, 17, 19: first charge coupling element, 18, 20: second charge Coupling elements, 9 and 13, 15 and 13, 17, 19 ... first reflection X
Line detecting means, 11 and 13, 16 and 13, 18,
20: second reflected X-ray detecting means, O: predetermined reference point, x
1: first distance, x2: second distance, Y: predetermined reference line.

──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-63-121737 (JP, A) JP-A-3-148056 (JP, A) JP-A-4-143642 (JP, A) JP-A-7-107 103919 (JP, A) Japanese Utility Model Hei 4-94557 (JP, U) (58) Field surveyed (Int. Cl. ⁶ , DB name) G01N 23/223

Claims (8)

(57) [Claims] 1. A sample fixed on a sample stage is irradiated with primary X-rays from an X-ray source also used for analysis, and at a first distance from a predetermined reference point in a traveling direction of the primary X-rays, A first intensity distribution in a height direction from a predetermined reference line is measured for the reflected X-rays reflected on the sample surface, and at a second distance from the reference point in a traveling direction of the primary X-ray, the reflection is measured. For X-rays, a second intensity distribution in the height direction from the reference line is measured. From the first and second intensity distributions, total reflection occurs on a sample surface immediately below an analysis detector used for analysis. In order to obtain such a deviation from the position of the sample stage, and to eliminate the deviation, the angle between the surface of the sample stage and the primary X-ray and the position of the sample stage below the detector for analysis are obtained. How to set the position of the sample stage in X-ray analysis to adjust the height from the reference line . 2. A sample stage on which a sample is fixed, an X-ray source which is also used for analysis and irradiates the sample with primary X-rays, and which is provided below an analytical detector used for analysis. An angle adjuster that adjusts an angle between the surface of the stage and the primary X-ray; a height adjuster that is provided below the analytical detector and adjusts the height of the sample stage from a predetermined reference line. And measuring a first intensity distribution in a height direction from the reference line at a first distance from a predetermined reference point in a traveling direction of the primary X-ray with respect to the reflected X-ray reflected on the sample surface. 1 reflected X-ray detecting means, and measuring a second intensity distribution of the reflected X-ray in a height direction from the reference line at a second distance from the reference point in a traveling direction of the primary X-ray. A second reflected X-ray detecting unit that performs the analysis detection based on the first and second intensity distributions. Control means for controlling the angle adjuster and the height adjuster so as to obtain a shift from the position of the sample stage such that total reflection occurs on the sample surface immediately below the instrument and eliminate the shift. Sample stage position setting device for X-ray analysis. 3. A sample fixed on a sample stage is irradiated with primary X-rays from an X-ray source also used for analysis, and at a first distance from a predetermined reference point in the direction of travel of the primary X-rays, A passage hole of a first shielding plate provided at a height such that total reflection X-rays immediately below the surface of the sample directly below the analysis detector used for analysis pass at a maximum intensity; At a second distance in the direction of travel of the X-rays, the reflection X reflected at the sample surface is passed through a passage hole of a second shielding plate provided at a height such that the total reflection X-rays immediately below pass at the maximum intensity. The angle formed between the surface of the sample table and the primary X-ray below the analytical detector and the sample table so that the intensity of the X-ray passes through and the intensity detected by the reflected X-ray detector is maximized. A method of setting the position of the sample stage in X-ray analysis for adjusting the height from a predetermined reference line. 4. A sample stage on which a sample is fixed, an X-ray source used also for analysis and for irradiating the sample with primary X-rays, and the sample provided below an analytical detector used for analysis. An angle adjuster that adjusts an angle between the surface of the stage and the primary X-ray; a height adjuster that is provided below the analytical detector and adjusts the height of the sample stage from a predetermined reference line. A reflected X-ray detector for detecting reflected X-rays reflected on the sample surface; and a sample surface immediately below the analytical detector at a first distance from a predetermined reference point in a traveling direction of the primary X-ray. A first shielding plate provided with a passage hole at a height such that total reflection X-rays immediately below the total reflection at the maximum pass therethrough, and a second distance from the reference point in the traveling direction of the primary X-rays , A second shielding plate provided with a passage hole at a height such that the total reflection X-ray directly below passes at a maximum intensity. The angle adjuster and the height so that the reflected X-rays pass through the through holes of the first and second shielding plates and the intensity detected by the reflected X-ray detector is maximized. An X-ray analyzer comprising: a control unit for controlling the adjuster. 5. A sample fixed on a sample stage is irradiated with primary X-rays from an X-ray source also used for analysis, and at a first distance from a predetermined reference point in a traveling direction of the primary X-rays, The reflected light reflected on the sample surface is passed through the passage hole of the first shielding plate provided at a height such that the total reflection X-ray directly below the sample surface directly below the analytical detector used for analysis passes at the maximum intensity. Adjust the height of the sample table from a predetermined reference line below the analytical detector so that the X-rays pass and the intensity detected by the reflected X-ray detector is maximized, At a second distance from the reference point in the traveling direction of the primary X-ray, the intensity distribution of the reflected X-ray in the height direction from the reference line is measured. To obtain a deviation from the position of the sample stage that causes Below the serial analytical detector, the sample stage position setting method of the X-ray analysis to adjust the angle and height from the sample stage of the reference line and the sample stage surface and the primary X-ray. 6. A sample stage on which a sample is fixed, an X-ray source also used for analysis and for irradiating the sample with primary X-rays, and a sample table provided below an analytical detector used for analysis. An angle adjuster that adjusts an angle between the surface of the stage and the primary X-ray; a height adjuster that is provided below the analytical detector and adjusts the height of the sample stage from a predetermined reference line. A reflected X-ray detector for detecting reflected X-rays reflected on the sample surface; and a sample surface immediately below the analytical detector at a first distance from a predetermined reference point in a traveling direction of the primary X-ray. A first shielding plate provided with a passage hole at a height such that total reflection X-rays immediately below the total reflection at the maximum pass therethrough, and a second distance from the reference point in the traveling direction of the primary X-rays A second shielding plate movable in a height direction from the reference line and provided with a passage hole; The height adjuster is controlled so that the reflected X-ray passes through the passage hole of the first shielding plate and the intensity detected by the reflected X-ray detector is maximized, and the control thereof is performed. For the later reflected X-rays, the sample that generates the directly-directed total reflection X-rays from the intensity distribution in the height direction from the reference line measured by the reflected X-ray detector and the second shielding plate. An apparatus for setting the position of a sample stage in X-ray analysis, comprising: control means for controlling the angle adjuster and the height adjuster so as to obtain a shift from the position of the stage and eliminate the shift. 7. The apparatus according to claim 2, wherein the first reflected X-ray detecting means moves in a height direction from the reference line at a first distance from the reference point in a traveling direction of the primary X-ray. A first shielding plate, which is freely provided with a passage hole, and a reflected X-ray detector for detecting the reflected X-ray, wherein the second reflected X-ray detecting means is one point away from the reference point. Next X
At a second distance in the traveling direction of the line, a second movable member provided with a passage hole and movable in the height direction from the reference line.
A position setting device for a sample stage in X-ray analysis, comprising: a shielding plate as described above; and the reflected X-ray detector. 8. The method according to claim 2, wherein the first reflected X-ray detecting means is a first charged coupling element for measuring the first intensity distribution, and wherein the second reflected X-ray detecting means is: A position setting device for a sample stage in X-ray analysis, which is a second charged coupling element for measuring the second intensity distribution.