JP2003344318A - Fluorescent x-ray analyzer - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To simply and easily prevent an analytical mechanism such as an irradiation source, a detector or the like from colliding with a sample in a fluorescent X-ray analyzer. <P>SOLUTION: In the fluorescent X-ray analyzer, a contact sensor used to detect that the sample S has come close to an irradiation chamber before the sample S collides with the analytical mechanism is installed, so as to prevent the analytical mechanism and the irradiation chamber from colliding with the sample. The X-ray analyzer comprises the irradiation source (an X-ray source 2) used to generate fluorescent X-rays from the sample, the irradiation chamber (an X-ray irradiation chamber 7) having the detector 6 used to detect the fluorescent X-rays, and a sample stage 8 arranged so as to face the irradiation chamber (the irradiation chamber 7) by keeping an interval at its lower part. A cover member 9 used to cover a face on which at least the irradiation chamber (the irradiation chamber 7) faces the sample stage 8 is provided between the irradiation chamber (the irradiation chamber 7) and the sample stage 8, and the cover member 9 constitutes an electrical switch mechanism used to detect its contact with the sample. <P>COPYRIGHT: (C)2004,JPO

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a fluorescent X-ray analyzer, and more particularly to prevention of collision of a sample.

[0002]

2. Description of the Related Art There is known a fluorescent X-ray analyzer for qualitative or quantitative analysis of a sample by irradiating the sample with X-rays and measuring the fluorescent X-rays generated from the sample with a detector. There is.

As one configuration of such a fluorescent X-ray analyzer, a sample stage is provided with an irradiation source equipped with an irradiation source for irradiating a sample with X-rays and an analysis mechanism such as a detector for detecting fluorescent X-rays generated from the sample. The X-ray is irradiated to the sample placed on the sample stage, and the fluorescent X-ray generated from the sample is detected.

In the fluorescent X-ray analyzer having this configuration, the sample is placed on the sample stage, and the sample stage is moved in the X and Y directions with respect to the irradiation chamber so that the irradiation position of the X-ray irradiation line is changed. The irradiation X-rays and the focus of the detector are adjusted to a predetermined height of the sample by adjusting the sample stage to a predetermined position on the plane and moving the sample stage in the Z direction (vertical direction) with respect to the irradiation chamber. Adjusted to fit.

[0005]

In the fluorescent X-ray microscope having the above-mentioned structure, the sample stage is moved up and down while the sample is placed on the sample stage, and the distance between the irradiation chamber and the sample is adjusted. Adjusting the focus position of the line. The adjustment of the focus position is usually performed with reference to the height of the sample stage itself. Therefore, when the sample stage is moved upward so as to approach the irradiation chamber side or laterally moved, the sample may collide with a part of the irradiation chamber depending on the thickness of the sample.

Since the conventional fluorescent X-ray microscope does not have a sample collision prevention mechanism, the sample arranged on the sample stage collides with the analysis mechanism and the irradiation chamber arranged above the sample stage, and the sample is damaged or damaged. There is a problem that the analysis mechanism and the irradiation chamber may be damaged.

In order to solve such a problem, the height of the sample surface is measured and the movement amount of the sample stage is controlled so that the sample does not collide with the analysis mechanism or the irradiation chamber. Although it is possible to prevent collision with the chamber, control of the sample stage is not always easy due to unevenness and inclination of the sample surface, or inclination of the sample stage itself, and a mechanism for measuring the surface height. And a complicated structure such as a control mechanism are required, which also causes a cost increase.

[0008] Therefore, the present invention solves the above-mentioned conventional problems, and in the fluorescent X-ray analyzer, an analysis mechanism such as an irradiation source and a detector, or an irradiation chamber, can be easily prevented from colliding with the sample. And

[0009]

The present invention provides a contact sensor for detecting that a sample approaches the irradiation chamber before the sample collides with the analysis mechanism, so that the analysis mechanism and the irradiation chamber collide with the sample. A sample stage that is arranged to face the irradiation chamber having an irradiation source for generating fluorescent X-rays from the sample and a detector for detecting the fluorescent X-rays, and a space below the irradiation chamber with a space therebetween. In the X-ray fluorescence analyzer having the above, a cover member is provided between the irradiation chamber and the sample stage to cover at least the surface of the irradiation chamber facing the sample stage, and the cover member constitutes an electrical switch mechanism.

By disposing the cover member of the present invention between the irradiation chamber and the sample stage, it is possible to prevent the sample arranged on the sample from directly contacting the irradiation chamber, and also to provide an electrical switch mechanism. With the configuration, it is possible to detect that the sample approaches the irradiation chamber. One end point of the electric switch mechanism can be a cover member, and the other end point can be an irradiation chamber or another independent contact member.

When the end points constituting the electrical switch mechanism are the cover member and the irradiation chamber, the cover member hangs downward from the irradiation chamber and hangs down to electrically separate the cover member and the normally open switch. Constitute. The electric switch mechanism is closed by raising the cover member and making contact with the irradiation chamber. This detects that the sample has come into contact with the cover member. On the other hand, when the cover member descends and separates from the analysis mechanism, the switch is opened, and it is detected that the contact between the sample and the cover member is released.

The electrical switch mechanism according to the present invention can have a simple structure in which a cover member is provided between the sample stage and the irradiation chamber to cover at least the surface of the irradiation chamber facing the sample stage.

Further, the sample stage is vertically moved (Z direction).
In addition to moving to the horizontal direction (X direction, Y direction), the sample can be detected as long as it contacts the cover member. Further, the X-ray fluorescence analyzer of the present invention is
The movement of the sample stage can be stopped based on the detection by the electrical switch mechanism.

[0014]

BEST MODE FOR CARRYING OUT THE INVENTION Embodiments of the present invention will be described in detail below with reference to the drawings. FIG. 1 is a schematic diagram for explaining a first mode of the X-ray fluorescence analyzer of the present invention. In the first form, an electric switch mechanism for detecting contact with a sample is composed of a cover member and an X-ray irradiation chamber.

The X-ray fluorescence analyzer 1 is configured to irradiate a sample S with X-rays, an X-ray source 2, an X-ray condensing capillary lens 3, and a capillary fixing that holds this capillary lens at a predetermined position. Equipped with a flange 4 for the sample S
As a configuration for detecting the fluorescent X-rays generated from, the fluorescent X-ray condensing unit 5 and the detector 6 are provided, and an analysis mechanism is configured. X
The radiation irradiation chamber 7 holds this analysis mechanism in a predetermined positional relationship,
At the opening of the X-ray irradiation chamber 7, the respective tip portions of the X-ray focusing capillary lens 3 and the fluorescent X-ray focusing section 5 are provided so as to project.

A sample stage 8 is provided below the X-ray irradiation chamber 7. The sample stage 8 has a sample S on the upper surface.
Are arranged and supported, and are movable in the X, Y and Z directions. It should be noted that the movement in the X and Y directions is performed by the sample S.
Is moved laterally with respect to the analysis mechanism, and the movement in the Z direction moves the sample S vertically with respect to the analysis mechanism.

The X-ray fluorescence analyzer 1 of the present invention is equipped with a cover member 9 in the gap between the X-ray irradiation chamber 7 and the sample stage 8. The cover member 9 covers at least the lower end portion of the X-ray irradiation chamber 7 to protect the sample S from directly contacting the tip portion of the X-ray focusing capillary lens 3 or the fluorescent X-ray focusing unit 5, and By combining with the X-ray irradiation chamber 7, an electric switch mechanism for detecting the contact of the sample S is constructed.

The electrical switch mechanism is composed of a circuit having the X-ray irradiation chamber 7 and the cover member 9 as contacts. In the normal state, the X-ray irradiation chamber 7 and the cover member 9 are in a non-contact state, and the circuit is in an open state. On the other hand, when the X-ray irradiation chamber 7 and the cover member 9 come into contact with each other, the circuit is closed. Therefore, by opening / closing this circuit, contact or non-contact between the X-ray irradiation chamber 7 and the cover member 9 can be detected, and further, the sample S may approach the X-ray irradiation chamber 7 and collide with it. Can be detected.

The cover member 9 is attached to the X-ray irradiation chamber 7 by a holding member 10 so as to be vertically movable in an electrically insulated state. The attachment of the cover member 9 by the holding member 10 can be performed, for example, by suspending the cover member 9 from the holding member 9 with an insulating screw member. In this suspension, the cover member 9 is provided with a margin in the vertical direction so that the cover member 9 can freely move up and down. Due to this suspended holding, when the sample S is not in contact with the cover member 9, the cover member 9 is held in a state of being lowered to the lower position by its own weight. At this time, a gap is formed between the upper surface of the cover member 9 and the lower end surface of the X-ray irradiation chamber 7, and the X-ray irradiation chamber 7 and the cover member 9 are electrically insulated. FIG. 1 (a) shows this state.

The sample is fixed on the sample stage, and the analysis position is moved to the focusing position of the X-ray focusing capillary lens using the sample stage. In this movement, when the sample stage 8 is moved upward (Z direction), when the unevenness of the sample is large, or when the sample moves above the analysis position, the sample S comes into contact with the cover member 9. As a result, the cover member 9 is pushed upward (in the Z direction) by the sample S, and the upper surface of the cover member 9 and the lower end surface of the X-ray irradiation chamber 7 come into contact with each other. When the upper surface of the cover member 9 and the lower end surface of the X-ray irradiation chamber 7 come into contact with each other, the circuit having the cover member 9 and the X-ray irradiation chamber 7 as a contact is closed. When this circuit is closed,
It can be detected by a detection means (not shown). Figure 1
(B) shows this state.

In the cover member 9, an opening 9a is formed in each extension of the X-ray condensing capillary lens 3 and the fluorescent X-ray condensing unit 5, and the X-ray condensing capillary lens 3 is used. The sample S is irradiated with the condensed X-rays, and the fluorescent X-rays emitted from the sample S by the X-ray irradiation are introduced into the fluorescent X-ray condensing unit 5.

The detecting means can be composed of a power source 11 and a detector 12 connected in a circuit as shown in FIG. 2, for example.

FIG. 2 is a diagram for explaining a circuit configuration for detecting contact between the cover member and the X-ray irradiation chamber. Figure 2
(A) shows a non-contact state between the cover member and the X-ray irradiation chamber. In this state, the cover member 9 is lowered to the lower position by its own weight, and a gap is formed between the cover member 9 and the X-ray irradiation chamber 7. Therefore, the power source 11, the cover member 9, X
The circuit formed by the line irradiation chamber 7 and the detector 12 is in an open state. This open state can be known by, for example, the voltage value or current value detected by the detector 12.

Next, when the sample stage 8 moves upward (Z direction) and the sample S on the sample stage rises excessively with this movement, the upper end of the sample S contacts the lower surface of the cover member 9. FIG. 2B shows a state in which the sample S and the cover member 9 are in contact with each other. In this state, since there is still a gap between the cover member 9 and the X-ray irradiation chamber 7, a closed circuit is not formed and no output appears in the detector 12.

When the sample stage 8 moves further upward (Z direction) and the sample S on the sample stage further rises with this movement, the cover member 9 is pushed up by the sample S, and the upper end surface of the cover member 9 is X-rayed. It contacts the lower surface of the irradiation chamber 7. Figure 2
(C) shows the state where the cover member 9 and the X-ray irradiation chamber 7 are in contact with each other. In this state, the cover member 9 and the X-ray irradiation chamber 7 are in contact with each other to form a closed circuit, and an output appears on the detector 12. As a result, it is detected that the sample S has approached the X-ray irradiation chamber 7.

The signal detected by the detector 12 is sent to control means (not shown) to control the sample stage 8. Examples of control modes of the sample stage 8 include stopping the sample stage and moving the sample stage downward.

Next, a second embodiment of the X-ray fluorescence analyzer of the present invention will be described with reference to FIG. In the second mode, the electrical switch mechanism for detecting contact with the sample is composed of the cover member, the X-ray irradiation chamber, and another independent contact member, and the sample is in contact with the cover member. The circuit is closed when there is no contact, and the circuit is opened when the sample is in contact with the cover member. In addition, in FIG.
Only part of the X-ray fluorescence analyzer is shown.

In FIG. 3, in the circuit constituting the detecting means, one end point is a cover member 9 and the other end point is a contact member 13 independent of the X-ray irradiation chamber 7, and the cover member 9 and the contact member 13 are connected to each other. The power source 11 and the detector 12 are connected between the two.

FIG. 3A shows a non-contact state between the cover member and the X-ray irradiation chamber. In this state, the cover member 9
Is lowered to its lower position by its own weight and is in contact with the contact member 13. Therefore, the circuit formed by the power source 11, the cover member 9, the contact member 13, and the detector 12 is in a closed state. This closed state can be known by, for example, the voltage value or current value detected by the detector 12.

Next, when the sample stage 8 moves upward (Z direction) and the sample S on the sample stage rises excessively with this movement, the upper end of the sample S comes into contact with the lower surface of the cover member 9. FIG. 3B shows a state where the sample S and the cover member 9 are in contact with each other. In this state, since the cover member 9 and the contact member 13 are in contact with each other, the closed circuit is still formed and the output of the detector 12 does not change.

When the sample stage 8 moves further upward (Z direction) and the sample S on the sample stage further rises with this movement, the cover member 9 is pushed up by the sample S and separated from the contact member 13. FIG. 3C shows a state in which the cover member 9 is separated from the contact member 13. In this state, the closed circuit is not formed because the contact between the cover member 9 and the contact member 13 is lost, and the output of the detector 12 changes. As a result, the sample S is transferred to the X-ray irradiation chamber 7
Is approached.

Next, contact detection when the sample stage moves laterally (X, Y directions) will be described with reference to FIG. In this contact detection, a part of the sample comes into contact with the cover member, and the contact between the cover member and the X-ray irradiation chamber is detected.

FIG. 4A shows a non-contact state between the cover member and the X-ray irradiation chamber. In this state, the cover member 9
Is lowered to the lower position by its own weight, and the X-ray irradiation chamber 7
And a gap is formed between the cover member 9 and the X-ray irradiation chamber 7 also in the lateral direction. As a result, the circuit formed by the power source 11, the cover member 9, the X-ray irradiation chamber 7, and the detector 12 is in an open state. This open state can be known by, for example, the voltage value or current value detected by the detector 12.

Next, when the sample stage 8 moves laterally (in the X and Y directions) and the sample S on the sample stage is excessively laterally displaced in accordance with this movement, the protrusion 14 of the sample S causes the protrusion 14 of the cover member 9 to move. Contact the sides. FIG. 4B shows a state in which the protrusion 14 of the sample S and the side surface of the cover member 9 are in contact with each other. In this state, the cover member 9 and the X-ray irradiation chamber 7
Since there is still a gap between and, a closed circuit is not formed and no output appears at the detector 12.

When the sample stage 8 is further moved in the lateral direction (X, Y directions) and the sample S on the sample stage is further laterally displaced due to this movement, the cover member 9 is pushed by the sample S and the cover member 9 is moved. The side portion 9a of the contact part comes into contact with the side surface of the X-ray irradiation chamber 7. FIG. 4C shows a state in which the side portion 9a of the cover member 9 and the side surface of the X-ray irradiation chamber 7 are in contact with each other. In this state, the cover member 9 and the X-ray irradiation chamber 7 are in contact with each other to form a closed circuit, and an output appears on the detector 12. As a result, it is detected that the sample S has approached the X-ray irradiation chamber 7.

Although the example shown in FIG. 4 shows the configuration shown in FIG. 2, the configuration shown in FIG. 3 can also be applied by appropriately disposing the contact members.

As described above, according to the present invention,
In the fluorescent X-ray analyzer, it is possible to easily prevent the collision between the analysis mechanism such as the irradiation source and the detector and the sample.

[0037]

[Brief description of drawings]

FIG. 1 is a schematic diagram for explaining a first mode of an X-ray fluorescence analyzer of the present invention.

FIG. 2 is a diagram for explaining a circuit configuration for detecting contact between the cover member and the X-ray irradiation chamber of the present invention.

FIG. 3 is a schematic diagram for explaining a second mode of the X-ray fluorescence analyzer of the present invention.

FIG. 4 is a diagram for explaining lateral contact between the cover member of the present invention and the X-ray irradiation chamber.

[Explanation of symbols]

1 ... Fluorescent X-ray analyzer, 2 ... X-ray source, 3 ... Capillary lens for collecting X-rays, 4 ... Capillary fixing flange, 5 ...
X-ray fluorescence condensing tube, 6 ... Detector, 7 ... X-ray irradiation chamber, 8 ... Sample stage, 9 ... Cover member, 9a ... Side part, 10 ... Holding member, 11 ... Power supply, 12 ... Detector, 13 ... Contact member, 1
4 ... Projection, S ... Sample.

Claims (4)

[Claims] 1. An irradiation chamber having an irradiation source for irradiating a sample with X-rays and a detector for detecting X-rays generated from the sample,
In a fluorescent X-ray analysis apparatus having a sample stage arranged below the irradiation chamber so as to face each other with a gap, a cover covering at least a surface of the irradiation chamber facing the sample stage between the irradiation chamber and the sample stage. An X-ray fluorescence analyzer, comprising a member, wherein the cover member constitutes one end of an electrical switch mechanism for detecting contact with a sample. 2. The X-ray fluorescence analyzer according to claim 1, wherein the other end of the electrical switch mechanism that comes into contact with the cover member is the irradiation chamber. 3. The electrical switch mechanism forms a normally open switch by electrically separating the cover member by hanging it from the irradiation chamber, and is closed by contact with the irradiation chamber when the cover member rises. The fluorescent X-ray analysis device according to claim 2, wherein 4. The X-ray fluorescence analyzer according to claim 1, wherein movement of the sample stage is stopped based on detection by the electrical switch mechanism.