JP2001021510A - X-ray analysis apparatus - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an X-ray analysis apparatus, capable of surely observing a sample and performing desired X-ray analysis even when the sample cannot be observed easily with an ordinary optical microscope. SOLUTION: In this X-ray analysis apparatus to irradiate a sample 13, which is mounted on a sample stage 12, with X rays, a fluorescence microscope or a differential interfence microscope is installed on the sample stage 12, and when the X rays irradiate the sample 13, the sample 13 is observed with the fluorescence microscope or the differential interfence microscope, and then the image data are fetched as an image data into a computer and are displayed on a display screen.

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 used for examining, for example, elements contained in a sample, their amounts, and their distribution.

[0002]

2. Description of the Related Art An X-ray analyzer irradiates, for example, a sample placed on a sample table with X-rays and detects fluorescent X-rays or transmitted X-rays generated at that time by a detector. By appropriately processing the detection output, it is possible to analyze the constituent elements and the internal structure of the sample.

By the way, when performing measurement using the above X-ray analyzer, it is necessary to specify in advance the measurement location (the location to be irradiated with X-rays) in the sample before irradiating the sample with X-rays. Conventionally, as shown in FIG. 3, X-rays (primary X-rays) are applied to a sample 52 placed on a sample stage 51.
Line) 53, the sample 52 is observed by an optical microscope or a CCD camera 54 from a direction different from that of the sample 53, and a measurement point is indicated by a laser pointer (not shown), or a cross marker (not shown) is superimposed on the obtained image. As shown. In FIG. 3, 55 is an X-ray generator, 5
6 is an X-ray conduit for guiding the X-rays 53 toward the sample, 57 is a fluorescent X-ray detector for detecting fluorescent X-rays 58 generated by irradiating the sample 52 with primary X-rays 53, 59 is a lens, 6
Reference numeral 0 denotes a light guide that guides visible light emitted to the sample 52.

[0004]

However, in the above-mentioned conventional X-ray analyzer, the sample is observed in a so-called bright field using a normal optical microscope, and the observation of the sample uses the intensity of visible light. For this reason, it was difficult to clearly observe a sample that emits fluorescence. For extremely fine structures in the sample,
In some cases, observation is not possible because of the resolution. That is, since the resolution in the optical microscope is determined by the numerical aperture of the objective lens, when observing a fine structure, it is necessary to use a large objective lens.
Therefore, the configuration of the X-ray analyzer becomes large.

[0005] The present invention has been made in consideration of the above-mentioned matters, and its object is to ensure that even a sample which is difficult to observe with a normal optical microscope can be observed, and a desired sample can be obtained. An object of the present invention is to provide an X-ray analyzer capable of performing X-ray analysis.

[0006]

In order to achieve the above object, the present invention provides an X-ray analyzer for irradiating a sample placed on a sample stage with X-rays. A fluorescent microscope or a differential interference microscope is provided above, and when irradiating the sample with X-rays, the sample is observed with the fluorescent microscope or the differential interference microscope and taken into a computer as image data, and the image data is displayed on a display screen of the computer. A sample image is displayed on the top (claim 1).

[0007] In the X-ray analyzer, a measurement position on the sample may be specified by designating a position on the sample image.

[0008]

1 and 2 show one embodiment of the present invention. First, in FIG.
Is a main body block of the X-ray analyzer, for example, made of brass, and an X-ray generator 3 containing an X-ray tube 2 and the like above the main block.
Is provided. 4 is a main body block 1 and an X-ray generator 3
This is a seal part interposed between the first and second members. Reference numeral 5 denotes a space in the main body block 1, in which an X-ray conduit 6 for guiding the primary X-ray a emitted from the X-ray generator 2 to an appropriate beam diameter is provided in the vertical direction. Have been.
Reference numeral 7 denotes an X-ray shielding wall connected to a lower portion of the main body block 1, which is made of, for example, stainless steel or lead glass.
A sample chamber 9 partitioned by a thin diaphragm 8 made of a line-permeable material
Are formed. Reference numeral 10 denotes a sample chamber entrance formed on the front side (left side in the drawing) of the X-ray shielding wall 7 for sample insertion / removal, and an opening / closing door 1 which rotates vertically.
1 is provided.

Reference numeral 12 denotes a sample table on which a sample 13 is placed.
Although the details of the sample stage 12 will be described later, the sample stage 12 moves the inside of the sample chamber 9 in the X direction, which is the width direction of the sample chamber 9, as shown in FIG. Direction), the Y direction (the left-right direction in FIG. 1), which is the depth direction of the sample chamber 9, and the Z direction (the up-down direction in FIG. 1), which is the height direction of the sample chamber 9, respectively. Hereinafter, a sample transfer stage 14 for holding and transferring the sample table 12 in a predetermined state will be described with reference to FIG.

First, reference numeral 15 denotes a base member which is rectangular in plan view and is provided from the front side (the sample chamber inlet 10 side) to the rear side (the right side in FIG. 1) so as to be longer in the Y direction. One end in the direction is held by an up-down drive mechanism 16 so that it can move in the up-down direction (Z direction).

In FIG. 2, reference numerals 17 and 18 denote side plates erected on both sides of the base member 15 in the longitudinal direction, and a screw member 19 and guide members 20 and 21 are pivotally supported on these side plates 17 and 18. Or is held. That is,
The screw member 19 is provided on one side in the X direction of the base member 15 over substantially the entire length in the Y direction, and is coupled to a stepping motor 22 that rotates in both forward and reverse directions. The guide members 20 and 21 are provided on both sides of the base member 15 in the X direction over substantially the entire length in the Y direction.

Reference numeral 23 denotes a sample stage holder which holds the sample stage 12 and moves the sample stage 12 along the guide members 20 and 21 in the Y direction. The sample stage holder is rectangular in plan view, for example, and has a screw member 19 at one end in the X direction. A bracket portion 24 having a nut member (not shown) to be screwed and a guided portion (not shown) guided while being held by the guide member 20 is provided, and a guide member 21 is provided at the other end in the X direction. And a bracket portion 25 having a guided portion (not shown) which is guided while being held by the bracket.

Reference numerals 26 and 27 denote side plates which are erected on both sides of the sample holder 23 in the X direction.
A screw member 28 and guide members 29 and 30 are pivotally supported or held at 27. That is, the screw member 28
Is provided on one side in the Y direction of the sample holder 23 over substantially the entire length in the X direction, and is coupled to a stepping motor 31 that rotates in both the forward and reverse directions. In addition, the guide members 29 and 30 are
On the both sides in the Y direction over substantially the entire length in the X direction.

The sample table 12 has a rectangular shape in plan view, for example, and has a top surface on which the sample 13 can be held horizontally, and a screw member 2 on one end side in the Y direction.
8 and a bracket portion 32 having a guided portion (not shown) guided by being held by the guide member 29 while being guided by the guide member 29, and having a guide at the other end in the Y direction. A bracket portion 33 having a guided portion (not shown) guided while being held by the member 30 is provided.

In the sample transfer stage 14 having the above structure, the stepping motor 22 is operated to
The sample stage holder 23 is moved to a position on the sample chamber entrance 10 side (hereinafter, referred to as the sample room entrance
Between the sample mounting position) and the irradiation position of the primary X-ray a directly below the X-ray conduit 6 (hereinafter referred to as the X-ray irradiation position).
The sample table 12 can be moved in the X direction by operating the stepping motor 31 when the sample table holder 23 is at the X-ray irradiation position while being able to move in the Y direction.

In the sample transfer stage 14, secondary X-rays (not shown) such as fluorescent X-rays b and transmitted X-rays (not shown) generated when the sample 13 on the sample stage 12 is irradiated with the primary X-rays a. It goes without saying that each member is configured and assembled so as not to shield or attenuate X-rays.

Referring again to FIG. 1, reference numeral 33 denotes, for example, a fluorescent light X-ray b generated in the sample 13 when the sample 13 on the sample stage 12 located at the X-ray irradiation position is irradiated with the primary X-ray a. A fluorescent X-ray detector comprising a semiconductor detector, which is provided at the tip of a housing 34 connected to a tank (not shown) containing a cooling medium.

In FIG. 1, reference numeral 35 denotes an upper surface of the X-ray shielding wall 7, more specifically, a sample table which is located between the sample mounting position and the X-ray irradiation position and which is transported by the sample transfer stage 14. The windows formed at positions corresponding to the twelve transport paths are made of a material that transmits visible light and fluorescent light well. Above the window 35, for example, a plurality of fluorescent microscopes 36 are provided with one of the objective lenses 37 facing the window 35. As the fluorescence microscope 36, a commercially available one can be used. Reference numeral 38 denotes a CCD camera for observing a minute portion, which is provided above the fluorescence microscope 36.

In FIG. 1, reference numeral 39 denotes a computer having an image processing function for integrally controlling the entire X-ray analyzer. The computer 39 comprises, for example, a personal computer, and includes a color display 40 as an output device and a keyboard and mouse as input devices. (Not shown in the drawings), and exchanges signals with a signal processing unit (to be described later), and receives signals from the fluorescence microscope 36 and the CCD camera 38 to perform signal processing and control commands. Is output. Reference numeral 41 denotes a signal processing unit which transmits / receives signals to / from the personal computer 39, performs signal processing, and executes the X-ray generator 2 and the sample transfer stage 1 based on a command from the personal computer 39.
4 vertical drive mechanism 16 and stepping motor 22,
A signal for controlling the control signal 31 is output.

The operation of the X-ray analyzer having the above configuration will be described. The internal space 5 is set to, for example, 0.1 Torr or less, and the sample chamber 9 is set to the atmospheric pressure. The door 11 is opened, and an IC chip as a sample 13 is inserted into the sample
And placed on the sample stage 12 at the sample placement position. Then, after the height of the base member 15 is adjusted by operating the up-down driving mechanism 16 so that the IC chip 13 does not come into contact with the ceiling portion of the sample chamber 9 during the movement, the opening / closing door 11 is closed.

By rotating the stepping motor 22 in a predetermined direction, the sample stage holder 23 at the sample mounting position is
It is transferred in the direction of the line irradiation position. By this transfer, the IC chip 13 placed on the sample stage 12 on the sample stage holder 23 is moved.
Passes below the window 35 and is
The fluorescent image from the C chip 13 is taken in synchronization with this transfer. When the IC chip 13 arrives at the X-ray irradiation position, the fluorescent image of the entire IC chip 13 is taken into the personal computer 39 and displayed on the screen 40 a of the color display 40.
The fluorescent image of the C chip 13 is displayed.

Therefore, the person in charge of measurement (or the operator)
Searches for a site to be measured from the sample image on the display screen 40a, and specifies a measurement position with, for example, a mouse. IC corresponding to the position specified on this screen 40a
The sample holder 23 is moved so that the position on the chip 13 is located at the point where the primary X-ray a is irradiated. This movement is performed by appropriately operating the stepping motors 22 and 31. By irradiating the primary X-ray a from the X-ray generator 2 in this state, desired measurement can be performed.

In the above X-ray analyzer, while the sample table 12 on which the IC chip 13 is mounted is transferred from the sample mounting position to the X-ray irradiation position, a fluorescent image of the entire IC chip 13 is transferred to the personal computer 39. The measurement location on the IC chip 13 can be easily specified by designating the location in the fluorescence image on the display screen 40a of the personal computer 39 without searching for the measurement location again. be able to.

The present invention is not limited to the above-described embodiment. For example, as a secondary X-ray detector, a primary X-ray detector may be used.
A transmission X-ray detector that detects a transmission X-ray transmitted through the sample 13 when the line a is irradiated may be provided below the sample transfer stage 14.

The sample may be any one that emits fluorescent light. Therefore, the sample may be an organism other than an IC chip. Further, when observing a minute portion of the sample 13, the CCD camera 38 may be used together.

A differential interference microscope may be used instead of the fluorescence microscope 36. In this case, the fine structure of the sample 13 such as an IC chip can be observed well.

Further, it is not always necessary to partition the internal space 5 and the sample chamber 9 with a thin diaphragm 8. In the case where the thin diaphragm 8 is not provided and light elements such as Na, Mg, and Al are measured, the internal space 5 is required for each measurement.
In addition, the sample chamber 9 needs to be evacuated or purged with a gas (for example, He) that does not affect the measurement.

Instead of the stepping motors 22 and 31 in the sample transfer stage 14, another motor such as a servomotor with an encoder may be used. Further, the signal processing unit 41 may be provided in the personal computer 39.

[0029]

As described above, according to the present invention, a sample is detected by a fluorescence microscope or a differential interference microscope on a path for transferring the sample from the sample mounting position to the X-ray irradiation position, and the image data is obtained by computer. To
Since this image data is displayed as a sample image on a display screen of a computer, even if the sample is difficult to see with a normal microscope such as an optical microscope, it can be observed without fail, and X The irradiation position of the line can be easily confirmed, and the analysis position can be easily specified.

By designating the position in the sample image, the measurement position on the sample can be specified. Therefore, the X-ray irradiation position on the sample can be set quickly and accurately, and the efficiency can be improved. A measurement can be made.

[Brief description of the drawings]

FIG. 1 is a diagram schematically showing an overall configuration of an X-ray analyzer according to the present invention.

FIG. 2 is a diagram schematically showing a planar configuration of a sample transfer stage of the X-ray analyzer.

FIG. 3 is an explanatory diagram of a conventional technique.

[Explanation of symbols]

12: sample stage, 13: sample, 36: fluorescence microscope or differential interference microscope, 39: computer, 40a: display screen, a: X-ray.

 ────────────────────────────────────────────────── ─── Continuing on the front page (72) Inventor Toshikazu Maki 2nd Higashi-cho, Kichijoin-miya, Minami-ku, Kyoto, Kyoto Inside Horiba Seisakusho (72) Inventor Shintaro Kotani 2 Address F-term in Horiba, Ltd. (reference) 2G001 AA01 DA02 EA03 HA09 HA13 HA20 JA11 JA16 LA01 LA11 NA05 NA06 NA16 NA17 PA02 PA07 PA11 PA14 SA02 SA10 2H052 AA05 AA09 AF02 AF13 AF14 AF23 AF25

Claims (2)

[Claims] 1. An X-ray analyzer for irradiating a sample placed on a sample table with X-rays, wherein a fluorescence microscope or a differential interference microscope is provided above the sample table.
When irradiating the sample with the line, the sample is observed by the fluorescence microscope or the differential interference microscope and taken into a computer as image data, and the image data is displayed as a sample image on a display screen of the computer. X-ray analyzer. 2. An X-ray analyzer in which a sample placed on a sample stage is irradiated with X-rays, wherein a fluorescence microscope or a differential interference microscope is provided above the sample stage.
When irradiating the sample with the line, the sample is observed by the fluorescence microscope or the differential interference microscope and taken into a computer as image data, and the image data is displayed as a sample image on a display screen of the computer. An X-ray analysis apparatus characterized in that a measurement position in the sample can be specified by designating the following.