JP2912194B2 - X-ray analyzer - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an X-ray analyzer for irradiating a sample with primary X-rays and analyzing generated secondary X-rays.

[0002]

2. Description of the Related Art As a conventional X-ray analyzer, for example, there is an apparatus as shown in FIG. In this apparatus, a primary X-ray 2 generated from an X-ray source 1 is irradiated on a sample 4 fixed on a sample stage 3, and a secondary X-ray 5 generated from the sample 4 is diverged by a diverging slit 6 and curved. The light is incident on the spectroscopic element 7, is separated into desired characteristic X-rays 8, is focused by the light receiving slit 9, is incident on the detector 10, and its intensity is measured. Here, the sample 4 having a diameter of 30 mm is used as a standard, and the positions of the slits 6 and 9, the position of the curved spectral element 7, the area of the incident surface, and the like are determined from the size. A sample chamber 11 having an X-ray source 1 and a sample stage 4, a divergence slit 6, a curved spectroscopic element 7, a light receiving slit 9, and a detector 1 so as to satisfy the conditions thus determined.
The spectroscopic chamber 12 having 0 is connected and fixed.

In the analysis using this conventional apparatus, when the sample 4 to be analyzed is smaller than 30 mm in diameter, or when the portion of the sample 4 to be analyzed is smaller than 30 mm in diameter (hereinafter referred to as "to be analyzed comprehensively"). analysis plane surface, the area thereof is referred to as analysis area a), as shown in FIG. 13, the view restrictor diaphragm 13 having a suitable pore size corresponding to, the analysis area S ₁ between the sample 4 and the divergence slit 6 And only the secondary X-rays 5 generated from the analysis surface are passed through the hole. View limiting diaphragm 13, so that is according to the magnitude of the analytical area S _1, it has a plurality of different diameter of the hole.

[0004]

However, for example, the analysis area S ₁ when the visual field limiting diaphragm 13 is used as shown in FIG. 13 is different from the analysis area S ₁ when it is not used as shown in FIG.
_If it is one-fourth of ₀ (which is 225πmm ² from the diameter of 30 mm), the intensity of the secondary X-ray generated from the analysis surface is also reduced to one-fourth. On the other hand, the intensity of the secondary X-ray finally incident on the detector 10 is also proportional to the solid angle α that sees the divergence slit 6 from one point on the analysis surface. Field limiting diaphragm 1
There is no difference between the case where 3 is used and the case where it is not used as shown in FIG. After all, the view restriction diaphragm 13
Is used, the intensity of the secondary X-ray incident on the detector 10 becomes
It will be reduced by a factor of four. That is, when the analysis area S ₁ is reduced by using the view restriction diaphragm 13,
The intensity of the secondary X-rays incident on the detector 10 will decrease in proportion to the analysis area S _1, the intensity of the secondary X-rays analysis area S ₁ is obtained as the smaller it is insufficient, an accurate analysis It becomes difficult.

Accordingly, an object of the present invention is to provide an X-ray analyzer capable of performing accurate analysis without insufficient secondary X-ray intensity even if the analysis area is reduced.

[0006]

To achieve the above object, an X-ray analyzer according to claim 1 is an X-ray analyzer for generating primary X-rays.
A source, a sample stage on which the sample is fixed, a divergence slit for passing a secondary X-ray generated from the sample irradiated with the primary X-ray, and a secondary X-ray passing through the divergence slit are incident. An X-ray analyzer comprising a curved spectroscopic element and a detector on which the secondary X-ray diffracted by the curved spectroscopic element is incident, wherein a secondary unit having the divergent slit, the curved spectroscopic element and a detector And at least one of the primary unit having the X-ray source and the sample stage, along a path of the secondary X-rays generated from the sample, passing through the divergence slit, and going to the curved spectroscopic element, with respect to the other. A moving means for moving closer or farther is provided.

[0007] In order to achieve the above object, the X
A X-ray source for generating primary X-rays, a sample stage on which the sample is fixed, a diaphragm for passing secondary X-rays generated from the sample irradiated with the primary X-rays, An X-ray analyzer comprising: a detector to which a secondary X-ray passing through an aperture is incident; a secondary unit having the aperture and a detector; and a primary unit having the X-ray source and a sample stage. A moving means for moving at least one of them along the path of secondary X-rays generated from the sample, passing through the aperture, and going to the detector, with respect to the other.

[0008] In order to achieve the above object, the X
The X-ray analyzer includes an X-ray source that generates primary X-rays, a slit that allows secondary X-rays generated from the sample irradiated with the primary X-ray, and a secondary X-ray that has passed through the slit. An X-ray analyzer provided with an incident detector, wherein the slit is moved toward or away from the sample along a path of secondary X-rays generated from the sample, passing through the slit, and going to the detector. Equipped with transportation means, from one point on the analysis surface to the front
The solid angle looking into the slit is inversely proportional to the analysis area .

[0009]

According to the X-ray analyzer of the first aspect,
At least one of a secondary unit having a divergence slit, a curved spectral element and a detector and a primary unit having an X-ray source and a sample stage are generated from a sample, pass through the divergent slit, and travel toward the curved spectral element. Along the path of the secondary X-ray, it approaches or separates from the other according to the analysis area, so even if the analysis area decreases, the solid angle that looks into the divergence slit from one point on the analysis surface is inversely proportional to the analysis area And increase. Therefore, even if the analysis area is small, the intensity of the obtained secondary X-ray is not insufficient, and accurate analysis can be performed.

According to the X-ray analyzer of the present invention, at least one of a secondary unit having an aperture and a detector and a primary unit having an X-ray source and a sample stage are generated from a sample. Along the path of the secondary X-rays passing through the aperture to the detector, the secondary X-rays are moved toward or away from the other depending on the analysis area.
The solid angle at which the aperture is viewed from the point increases in inverse proportion to the analysis area. Therefore, even if the analysis area is small, the intensity of the obtained secondary X-ray is not insufficient, and accurate analysis can be performed.

According to X-ray analysis apparatus according to claim 3, the slit, and generated from the sample along the path of the secondary X-rays toward passing through the slit detector, since the closer or away from the sample, the analysis Even if the area decreases, the solid angle at which the slit is viewed from one point on the analysis surface increases in inverse proportion to the analysis area. Therefore, even if the analysis area is small, the intensity of the obtained secondary X-ray is not insufficient, and accurate analysis can be performed.

[0012]

Embodiments of the present invention will be described below with reference to the drawings. The X-ray analyzer according to the first embodiment of the present invention includes a primary unit 14, a secondary unit 15, a moving unit 16, and a metal bellows 17, as shown in FIG. The primary unit 14 has an X-ray source 1 for generating primary X-rays 2 and a sample stage 3 on which a sample 4 is fixed. The secondary unit 15 includes a divergence slit 6 for passing a secondary X-ray 5 generated from the sample 4 irradiated with the primary X-ray 2, and a curvature on which the secondary X-ray 5 passing through the divergence slit 6 is incident. It has a spectral element 7, a light receiving slit 9 for passing the secondary X-rays 8 diffracted by the curved spectral element 7, and a detector 10 to which the secondary X-rays 8 passed through the light receiving slit 9 are incident. .

The moving means 16 is screwed into a female screw part 22 provided on the upper part of the secondary unit 15 and has one ball screw 18 penetrating through the slide part 40. 2 penetrating through the provided slide portion 41
One slide shaft 19 (only one is shown), a motor 25 having a rotating shaft connected to one end of the ball screw 18, a mounting plate 20 to which the motor 25 and the like are mounted, and a motor 25 And control means 42 for appropriately rotating.

Each of the one ball screw 18 and the two slide shafts 19 is along the path of the secondary X-ray 5 generated from the sample 4 and passing through the diverging slit 6 toward the curved spectral element 7. As shown in FIG. 2 which is parallel to each other and is a view as viewed from the axial direction II, the centers of their end faces are arranged at the positions of the vertices of an isosceles triangle. Returning to FIG. 1, the male screw of the ball screw 18 is formed at about half of the motor 25 side except for the end, and one end of the male screw is rotatable to the support portion 20 of the primary unit 14 via the rotary bearing 21. And the slide bearing 24 provided on the slide portion 40 provided on the upper part of the secondary unit 15.
, And screwed into a female screw portion 22 provided on the upper part of the secondary unit 15, and the other end is rotatably supported by the mounting plate 20 via a rotary bearing 23, and the other end is connected to a motor 25. Is connected to the rotating shaft.

One end of the slide shaft 19 is fixed to the primary unit 14 by screwing or the like, and slide bearings 24 (only two left ones are shown) provided on the left and right sides of the secondary unit 15 are provided. And the other end is fixed to the mounting plate 20 by screwing or the like. With this configuration, the secondary unit 15 is movable along the ball screw 18 and the slide shaft 19 with respect to the fixed primary unit 14 by the rotation of the motor 25. The metal bellows 17 is tubular and flexible, and connects the primary unit 14 and the secondary unit 15 while maintaining airtightness even when the secondary unit 15 moves.

Next, the operation of the apparatus of the first embodiment will be described. For simplicity, only the optical system of this device is shown in FIG. When analyzing a sample 4 of a standard size having an analysis area S _0, the solid angle at which the divergence slit 6 is viewed from one point on the analysis surface is α, as in the conventional apparatus. Here, for example, when analyzing an analysis surface in which the analysis area S ₁ is a quarter of S ₀ , when a movement command signal is input to the control means 42 of FIG. In accordance with the program, the motor 25 is rotated by a fixed amount, and the secondary unit 15 is rotated along the ball screw 18 and the slide shaft 19, that is, the secondary unit 15 is generated from the sample 4 and passes through the divergence slit 6 toward the curved spectroscopic element 7. The primary unit 14 is approached along the path of the X-ray 5.

FIG. 4 shows only the optical system in this state. In this state, the intensity of the secondary X-ray generated from the analysis surface is 4
The point that the number is reduced by a factor of 1 is the same as that of the conventional apparatus. However, in the apparatus of the first embodiment, the analysis area S
_{Even if 1} is reduced to one-fourth of S _0, the solid angle β that sees the divergence slit 6 from one point on the analysis surface increases four times the α in inverse proportion to the analysis area. Intensity of the secondary X-rays incident to ultimately detector 10, because also proportional to the solid angle to expect divergence slit 6 from a point on the analytical surface, eventually, be analyzed area S ₁ is smaller, the detection The intensity of the secondary X-ray obtained in the vessel 10 does not change, and accurate analysis can be performed.

Next, a second embodiment of the present invention will be described. As shown in FIG. 5, the X-ray analyzer of the second embodiment
The primary unit 14, the secondary unit 26, the moving unit 27, and the metal bellows 17 are provided. The primary unit 14 has an X-ray source 1 for generating primary X-rays 2 and a sample stage 3 on which a sample 4 is fixed. The secondary unit 26 includes a stop 28 for passing the secondary X-rays 5 generated from the sample 4 irradiated with the primary X-rays 2 and a detector 29 to which the secondary X-rays 5 passing through the stop 28 are incident. And
The moving means 27 includes one ball screw 18 that is threaded through a female screw portion 30 provided above the detector 29,
9, two slide shafts 19 penetrating through a slide portion 31 provided at a lower portion, a motor 25 having a rotating shaft connected to one end of a ball screw 18, a mounting plate 32 to which the motor 25 and the like are mounted, a movement command Control means 42 for receiving the signal and rotating the motor 25 appropriately.

The one ball screw 18 and the two slide shafts 19 are both generated from the sample 4 and are
As shown in FIG. 6, which is along the path of the secondary X-rays 5 passing through and going to the detector 29 and being parallel to each other and viewed from their axial direction VI, the centers of their end faces are They are arranged at the positions of the vertices of an isosceles triangle. Returning to FIG. 5, a male screw is formed on the ball screw 18 except for both ends, and one end of the ball screw 18 is
It is rotatably supported by the support portion 20 of the next unit 14,
The other end is rotatably supported on a mounting plate 32 via a rotary bearing 23, and the other end is connected to the rotating shaft of a motor 25.

The slide shaft 19 has one end fixed to the primary unit 14 by a screw or the like, penetrates a slide portion 31 provided below the detector 29 through a slide bearing 24, and has the other end screwed. It is fixed to the mounting plate 32 by the like. With this configuration, the secondary unit 26
Is movable along the ball screw 18 and the slide shaft 19 with respect to the fixed primary unit 14 by the rotation of the motor 25. Metal bellows 17
Has a tubular shape and has flexibility, even if the secondary unit 26 moves, the primary unit 14 and the secondary unit 26
Connect while maintaining airtightness.

Next, the operation of the apparatus according to the second embodiment will be described. For simplicity, only the optical system of this device is shown in FIG. When analyzing a sample 4 of a standard size having an analysis area S _0, the solid angle at which the stop 28 is viewed from one point on the analysis surface is α. Here, for example, when analyzing an analysis surface in which the analysis area S ₁ is one-fourth of S ₀ , the movement command signal is manually input to the control means 42 of FIG. 25 is rotated by a fixed amount, and the secondary side unit 2
6 is brought closer to the primary unit 14 along the ball screw 18 and the slide shaft 19, that is, along the path of the secondary X-ray 5 generated from the sample 4, passing through the aperture 28 and going to the detector 29. .

FIG. 8 shows only the optical system in this state. In this state, the intensity of the secondary X-ray generated from the analysis surface is 4
The point that the number is reduced by a factor of 1 is the same as that of the conventional apparatus. However, in the apparatus of the second embodiment, even if the analysis area is reduced to one-fourth, the solid angle β that sees the stop 28 from one point on the analysis surface is inversely proportional to the analysis area and is four times the α. To increase. Since the intensity of the secondary X-ray finally incident on the detector 29 is also proportional to the solid angle at which the diaphragm 28 is viewed from one point on the analysis surface, even if the analysis area S ₁ eventually becomes smaller,
The intensity of the secondary X-ray obtained by the detector 29 does not change, and accurate analysis can be performed.

Next, a third embodiment of the present invention will be described. As shown in FIG. 9, the X-ray analyzer according to the third embodiment
First, an X-ray source 1 for generating a primary X-ray 2, a sample stage 3 on which a sample 4 is fixed, and a slit for passing a secondary X-ray 5 generated from the sample 4 irradiated with the primary X-ray 2 33 and a detector 34 to which the secondary X-ray 5 passing through the slit 33 is incident
And A moving means 35 for moving the slit 33 toward or away from the sample 4 along a path of the secondary X-ray 5 generated from the sample 4 and passing through the slit 33 toward the detector 34 is provided . Slit 33 from one point
The solid angles α and β (FIGS. 10 and 11) for which the analysis area S
₀ and S ₁ (FIGS. 10 and 11) .

The moving means 35 includes two linear motors 36 mounted on the device above and below the detector 34,
And control means 43 for receiving the movement command signal and appropriately expanding and contracting the rods 37 of the two linear motors 36.
The distal end of a rod 37 that can be extended and contracted in the axial direction of the linear motor 36 is fixed above and below a slit member 38 having a slit 33. With this configuration, the slit 33 is
Due to the simultaneous expansion and contraction of the rods 37 of the two linear motors 36, the slit 33 generated from the sample 4
Along the path of the secondary X-rays passing through
It is movable.

Next, the operation of the device according to the third embodiment will be described. For simplicity, only the optical system of this device is shown in FIG. When analyzing a sample 4 of a standard size having an analysis area S _0, the solid angle at which the slit 33 is viewed from one point on the analysis surface is α. Here, for example, the analysis area S ₁ is S ₀
When analyzing an analysis surface that is a quarter of
By manually inputting the movement command signal to the control means 43, the two rods 37 are simultaneously extended by a certain amount, and the slit 33 is generated from the sample 4, passes through the slit 33, and travels to the detector 34. The sample 4 is approached along the X-ray path.

FIG. 11 shows only the optical system in this state. In this state, the point that the intensity of the secondary X-ray generated from the analysis surface is reduced to one fourth is the same as that of the conventional apparatus. However, in the apparatus of the third embodiment, even if the analysis area is reduced to one-fourth, the slit 3 is moved from one point on the analysis surface.
The solid angle β for 3 is inversely proportional to the analysis area,
Increase by a factor of two. The intensity of the secondary X-rays incident to the final detector 34, because also proportional to the one point on the analytical surface solid angle looking into the slit 33, after all, be smaller analysis area S _1, the detector The intensity of the secondary X-ray obtained at 34 does not change, and accurate analysis can be performed.

In the first and second embodiments, the secondary unit 1 is fixed to the fixed primary unit 14.
5 and 26 were moved, but conversely, the secondary units 15 and 2 were moved.
6 may be fixed, and the primary unit 14 may be moved in response thereto. Further, the secondary X-rays 5 generated from the sample 4 to which the present invention is applied are not limited to fluorescent X-rays, but are also applicable to Compton scattered rays.

[Brief description of the drawings]

FIG. 1 is a schematic side partial sectional view showing an X-ray analyzer according to a first embodiment of the present invention.

FIG. 2 is a diagram showing an X-ray analyzer according to a first embodiment of the present invention.
FIG. 2 is a view in the direction of arrow II in FIG.

FIG. 3 is a schematic side view showing an optical system in the X-ray analyzer according to the first embodiment of the present invention when analyzing an analysis surface of a standard size.

FIG. 4 is a schematic side view showing an optical system in the X-ray analyzer according to the first embodiment of the present invention when analyzing an analysis surface smaller than a standard size.

FIG. 5 is a schematic side partial sectional view showing an X-ray analyzer according to a second embodiment of the present invention.

FIG. 6 is a diagram showing an X-ray analyzer according to a second embodiment of the present invention.
FIG. 6 is a view taken in the direction of arrows VI in FIG.

FIG. 7 is a schematic side view showing an optical system in an X-ray analyzer according to a second embodiment of the present invention when analyzing a standard size analysis surface.

FIG. 8 is a schematic side view showing an optical system in an X-ray analyzer according to a second embodiment of the present invention when analyzing an analysis surface smaller than a standard size.

FIG. 9 is a schematic side partial sectional view showing an X-ray analyzer according to a third embodiment of the present invention.

FIG. 10 is a schematic side view showing an optical system in an X-ray analyzer according to a third embodiment of the present invention when analyzing a standard-size analysis surface.

FIG. 11 is a schematic side view showing an optical system in an X-ray analyzer according to a third embodiment of the present invention when analyzing an analysis surface smaller than a standard size.

FIG. 12 shows a conventional X when analyzing a standard size analysis surface.
FIG. 2 is a schematic partial side sectional view showing a line analyzer.

FIG. 13 is a schematic partial side sectional view showing a conventional X-ray analyzer when analyzing an analysis surface smaller than a standard size.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... X-ray source, 2 ... Primary X-ray, 3 ... Sample stage, 4 ... Sample, 5
… Secondary X-rays generated from the sample, 6 divergent slits, 7…
Curved spectroscopic element, 8 ... Secondary X diffracted by the curved spectroscopic element
Wire, 10, 29 ... detector, 14 ... primary unit, 1
5, 26 ... secondary unit, 16, 27, 35 ... moving means, 28 ... stop, 33 ... slit.

──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int.Cl. ⁶ , DB name) G01N 23/22-23/227 G21K 1/06

Claims (3)

(57) [Claims] An X-ray source for generating primary X-rays, a sample stage on which a sample is fixed, a divergent slit for passing secondary X-rays generated from the sample irradiated with the primary X-rays, An X-ray analyzer, comprising: a curved spectroscopic element to which secondary X-rays passing through the diverging slit is incident; and a detector to which secondary X-rays diffracted by the curved spectroscopic element are incident. , A secondary unit having a curved spectroscopic element and a detector, and a secondary unit having the X-ray source and a sample stage.
At least one of the secondary unit and the secondary X is generated from the sample, passes through the divergence slit, and travels to the curved spectral element.
An X-ray analyzer comprising moving means for moving closer to or away from the other along a line path. 2. An X-ray source for generating primary X-rays, a sample stage on which a sample is fixed, an aperture for passing secondary X-rays generated from the sample irradiated with the primary X-rays, An X-ray analyzer comprising: a detector to which a secondary X-ray passing through a diaphragm is incident; a secondary unit having the diaphragm and a detector; and a primary unit having the X-ray source and a sample stage. X-ray analysis characterized by comprising moving means for moving at least one of the following along a path of secondary X-rays generated from the sample, passing through the aperture, and going to the detector, with respect to or away from the other. apparatus. 3. An X-ray source for generating a primary X-ray, a slit for passing a secondary X-ray generated from a sample irradiated with the primary X-ray, and a secondary X-ray passing through the slit. An X-ray analyzer comprising a detector to be incident, wherein the slit is moved toward or away from the sample along a path of a secondary X-ray generated from the sample, passing through the slit, and going to the detector. Equipped with transportation means, one point on the analysis surface
The solid angle to see the slit from is inversely proportional to the analysis area
X-ray analysis apparatus, characterized in that that.