JP4731749B2 - X-ray analyzer - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to elements and X-ray analysis equipment used to determine the amount and its distribution are included, for example, in the sample.
[0002]
[Prior art]
The X-ray analyzer, for example, irradiates a sample placed on a sample stage with X-rays, detects fluorescent X-rays or transmitted X-rays generated at that time with a detector, and appropriately detects the detection output. By processing, the constituent elements and internal structure of the sample are analyzed.
[0003]
By the way, when performing measurement using the X-ray analyzer, it is necessary to specify in advance a measurement location (a location where X-rays are irradiated) in the sample before the sample is irradiated with X-rays. Conventionally, as shown in FIG. 5, the sample 52 is observed by an optical microscope or a CCD camera 54 from a direction different from the X-ray (primary X-ray) 53 irradiated to the sample 52 placed on the sample stage 51. The measurement location is indicated by a laser pointer (not shown), or a cross marker (not shown) is superimposed on the obtained image. In FIG. 5, 55 is an X-ray generator, 56 is an X-ray conduit for guiding the X-ray 53 in the sample direction, and 57 is a fluorescent X-ray 58 generated by irradiation of the primary X-ray 53 onto the sample 52. A fluorescent X-ray detector to be detected, 59 is a lens, and 60 is a light guide that guides visible light applied to the sample 52.
[0004]
[Problems to be solved by the invention]
However, the conventional method has the following disadvantages. That is, if the lens 59 is made interchangeable or a smooth lens is used to make it easier to find the sample 52, the optical axis shifts and the cost increases.
[0005]
In the conventional method, the irradiation direction of the primary X-ray 53 on the sample 52 and the optical observation direction of the sample 52 are different, so that if the height of the sample 52 on the sample stage 51 changes, the optical image The irradiation position of the X-ray inside changes.
[0006]
Moreover, when adjustment is insufficient, an exact X-ray irradiation position is not known. In addition, there is a disadvantage that even if the initial adjustment is accurately performed, it is difficult to notice even if the irradiation position is shifted due to a disturbance such as a physical impact.
[0007]
The present invention has been made in consideration of the above-mentioned matters, and its purpose is to quickly and accurately confirm the X-ray irradiation position or irradiation region in the sample, and to perform measurement efficiently. it is to provide an analytical equipment.
[0008]
[Means for Solving the Problems]
In order to achieve the above object, according to the present invention, in an X-ray analyzer configured to irradiate a sample with X-rays from an X-ray source, X-rays are inserted between the X-ray source and the sample but visible. A visible light mirror that reflects light rays, and an X-ray conduit having a visible light guide portion that passes visible light around an X-ray guide portion that guides X-rays are provided, and the sample is irradiated with visible light rays. An optical image capturing unit for capturing an optical image of the sample obtained through the visible light guide portion and the visible light mirror is provided .
[0009]
According to the X-ray analyzer, the position or region where X-rays are irradiated can be reliably confirmed based on the optical image of the sample.
[0010]
As the X-ray conduit used in the X-ray analyzer of the present invention, a visible light guide part for guiding a visible light beam is formed around a plurality of optical fibers and an X-ray guide part for guiding the X-ray to the center part. In this way, a hollow X-ray guide part that guides X-rays is formed at the center of a thick glass rod, and a visible light guide part that guides visible light is formed around it. At the same time, one obtained by polishing both end faces of the glass rod (Claim 3) can be suitably used.
[0011]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, the details of the present invention will be described with reference to the drawings. FIG. 1 is a diagram schematically showing the configuration of the main part of the X-ray analyzer according to the present invention. In this figure, 1 is a horizontal sample stage for holding a sample 2 and is held in the X direction (on the paper surface) by a holding mechanism 3. It is configured to move linearly in the left-right direction), the Y-direction (direction perpendicular to the paper surface), and the Z-direction (up-down direction along the paper surface). An X-ray source 4 is provided above the sample stage 1 and includes an appropriate X-ray tube, a mechanism for narrowing the X-rays to a predetermined beam diameter (for example, a diameter of 100 μm), and the like. a is issued to the sample 2 on the sample stage 1.
[0012]
Reference numeral 5 denotes a fluorescent X-ray detector composed of, for example, a semiconductor detector for detecting the fluorescent X-ray b generated in the sample 2 when the sample 2 on the sample stage 1 is irradiated with the primary X-ray a. Is provided at the front end of the housing 6 connected to a tank (not shown) containing a cooling medium. Reference numeral 7 denotes a transmission X-ray detector that detects a transmission X-ray c transmitted through the sample 2 when the sample 2 is irradiated with the primary X-ray a, and is provided below the sample stage 1.
[0013]
An illumination device 8 appropriately illuminates the sample 2 on the sample stage 1 and includes a light source that emits visible light d.
[0014]
Between the X-ray source 4 and the sample 2 on the sample stage 1, a visible light mirror 9 and an X-ray conduit 10 are provided in series in this order. The visible light mirror 9 is configured to allow X-rays to pass therethrough but reflect visible light. In this embodiment, a visible light reflecting surface 11 is formed on one surface, and the center thereof is, for example, 100 μm. It consists of a pinhole mirror provided with a pinhole 12 through which X-rays a having a reduced diameter can pass. The visible light mirror 9 is interposed so that the visible light reflecting surface 11 faces the sample stage 1 and forms an inclination angle of, for example, 45 ° with the X-ray irradiation direction (irradiation optical axis 13). Yes.
[0015]
The X-ray conduit 10 includes a central X-ray guide portion 14 that guides the X-ray a, and a visible light guide that guides the visible light e from the sample 2 provided around the X-ray guide portion 14. In this embodiment, as shown in an enlarged view in FIG. 3, a large number of optical fibers 16 are appropriately bundled in a cylindrical sheath tube 17 made of an appropriate material and having an appropriate thickness. One optical fiber 16 located at the center is extracted, and the apertured portion after the extraction is finished to a smooth surface (mirror surface state) to form an X-ray guide portion 14. Therefore, the X-ray conduit 10 is provided in the vertical direction so that the X-ray guide portion 14 extends in the length direction at the center of the visible light guide portion 15 composed of a large number of optical fibers 16 and is parallel to the irradiation optical axis 13. It has been. Further, both end portions of the X-ray guide portion 14 and both end portions of the visible light guide portion 15 made up of a large number of optical fibers 16 are aligned with each other.
[0016]
The outer diameter per one of the optical fibers 16 is, for example, several μm, and the inner diameter of the X-ray guide portion 14 is, for example, 100 μm. The X-ray conduit 10 has a diameter of 15 mm and a length of 140 mm, for example. Such an X-ray conduit 10 is arranged such that the X-ray guide portion 14 is concentric with the pinhole 12 of the visible light mirror 9. In addition, as what accommodated the said many optical fibers 16 in the state bundled in the sheath pipe 17, there exists a fiber optics plate (FOP) made from Hamamatsu Photonics, for example.
[0017]
In this embodiment, a slight gap (for example, about several mm to 1 cm) is formed between the lower end surface of the X-ray conduit 10 and the sample 2, and the optical image of the visible light guide unit 15 is formed. Since the image is blurred, a condensing lens 18 such as a convex lens is interposed in the gap to prevent the image from blurring. FIG. 2 is an enlarged view of a portion where the condenser lens 18 is interposed. In the illustrated example, the condenser lens 18 is provided approximately in the middle between the lower end surface of the X-ray conduit 10 and the surface of the sample 2. However, it is not limited to this. An X-ray guide hole 19 that allows X-rays a to pass therethrough is formed in the center of the condenser lens 18 in the thickness direction.
[0018]
In FIG. 1 again, reference numeral 20 denotes an optical image capturing unit provided on the reflection optical axis 21 (perpendicular to the irradiation optical axis 13) of the visible light mirror 9, and the illumination device 8 illuminates the sample 2 with visible light d. In this case, the optical image of the sample 2 is taken in, and is composed of, for example, an optical microscope or a CCD camera.
[0019]
An arithmetic control unit 22 controls the entire apparatus or processes the output signals of the detectors 5 and 7 and the image signal from the optical image capturing unit 20, and is composed of, for example, a computer having an image processing function. Color display 23 and a keyboard and mouse (both not shown) as input devices.
[0020]
The operation of the X-ray analyzer having the above configuration will be described. Prior to the irradiation of the sample 2 with the X-ray a, the X-ray irradiation position or irradiation region in the sample 2 is confirmed as follows. That is, X-ray a is emitted from the X-ray source 4 to, for example, the center of the sample 2 placed on the sample stage 1, and visible light d is emitted by the illumination device 8. Thus, the X-ray a irradiates the sample 2 through the X-ray guide portion 14 of the X-ray conduit 10 and the X-ray guide hole 19 of the condenser lens 18 through the pinhole 12 of the visible light mirror 9. On the other hand, visible light d from the illumination device 8 irradiates the entire surface of the sample 1.
[0021]
Then, the visible light e from the sample 2 irradiated on the entire surface by the visible light d enters the visible light guide unit 15 through the condenser lens 18, and is further reflected by the visible light mirror 9 to be an optical image capturing unit. 20 and displayed on the screen 23a of the color display 23 of the computer 22 in a state where an optical image of the entire sample 2 as shown by reference numeral 24 is enlarged at a predetermined magnification. At this time, an area as indicated by reference numeral 25 is enlarged and displayed at the same magnification almost at the center of the optical image 24. This region 25 indicates the irradiation position of the X-ray a with respect to the sample 2. That is, when X-ray a and visible light d are simultaneously irradiated onto the sample 2, the irradiation position of the X-ray a is a portion (region) 25 that is missing at a predetermined size in the optical image 24 of the sample 2. Therefore, the irradiation position or irradiation region of the X-ray a with respect to the sample 2 can be confirmed by visually confirming the position of the missing portion 25. After confirming the irradiation position or irradiation area, a predetermined X-ray analysis is performed.
[0022]
Note that the optical image 24 does not necessarily display the entire sample 2 and may be partially enlarged.
[0023]
As described above, in the X-ray analyzer configured as described above, the irradiation position or region of the X-ray a on the sample 2 can be reliably confirmed based on the optical image 24 of the sample 2, and the irradiation position of the X-ray a. Or the irradiation area can always be grasped reliably. And since no adjustment is required for the confirmation of the irradiation position or the irradiation region, the confirmation operation can be performed very easily.
[0024]
In the above embodiment, the condensing lens 18 is interposed between the lower end surface of the X-ray conduit 10 and the sample 2 to prevent the optical image of the sample 2 from blurring. When the gap between the lower end surface of the wire conduit 10 and the sample 2 is set to be close to 1 mm or less, the installation of the condenser lens 18 can be omitted. Preferably, the lower end surface of the X-ray conduit 10 and the sample 2 are preferably brought into close contact with each other. In this case, the sample 2 is irradiated with visible light d from below the sample stage 1. There is a need to.
[0025]
The present invention is not limited to the above-described embodiment, and the X-ray conduit 10 shown in FIG. 4 may be used. That is, in this figure, reference numeral 26 denotes an X-ray conduit made of a glass rod 27 having an appropriate diameter and an appropriate length, and a hollow portion 28 is formed so as to longitudinally cut the central portion in the length direction. The portion 28 is finished smoothly (in a mirror state) to form an X-ray guide portion, and a guide portion 29 that allows visible light to pass around the X-ray guide portion 28. Note that both end surfaces 27a and 27b in the length direction of the glass rod 27 are polished so as to be in a mirror state.
[0026]
Further, the visible light mirror 9 is not limited to the pinhole mirror, and may be formed of, for example, Be (beryllium) having a property that allows X-rays to pass through the mirror body but not visible light.
[0027]
【The invention's effect】
In the X-ray analyzer of the present invention, the position or region irradiated with X-rays can be reliably confirmed based on the optical image of the sample, and no adjustment is required for the confirmation. The confirmation work can be performed very easily and quickly.
[0028]
The X-ray conduit used in the X-ray analyzer of the present invention has a simple structure, is easy to handle, and is easy to manufacture. Therefore, it is preferably used as an X-ray guide member in the X-ray analyzer. be able to.
[Brief description of the drawings]
FIG. 1 is a diagram schematically showing a configuration of a main part of an X-ray analyzer according to the present invention.
FIG. 2 is a partially enlarged view showing a positional relationship among a sample, an X-ray conduit, and a condenser lens in the X-ray analyzer.
FIG. 3 is an enlarged perspective view showing an example of an X-ray conduit incorporated in the X-ray analyzer.
FIG. 4 is an enlarged perspective view showing another example of the X-ray conduit.
FIG. 5 is an explanatory diagram of a prior art.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 2 ... Sample, 4 ... X-ray source, 9 ... Visible light mirror, 10 ... X-ray conduit | pipe, 14 ... X-ray guide part, 16 ... Visible light guide part, 17 ... Optical fiber, 20 ... Optical image capture unit, 24 ... Sample 26 ... X-ray conduit, 27 ... glass rod, 27a, 27b ... end face, 28 ... X-ray guide part, 29 ... visible light guide part, a ... X-ray, d ... visible light, e ... visible light.

Claims (3)

In an X-ray analyzer configured to irradiate a sample with X-rays from an X-ray source, a visible light mirror that allows X-rays to pass but reflects visible light between the X-ray source and the sample, and an X-ray an X-ray guide unit X-ray conduit visible light guide portion for passing the visible light is formed on the periphery of the guide is provided, further, the visible light guide portion and visible light in when irradiated with visible light to said sample An X-ray analyzer comprising an optical image capturing unit for capturing an optical image of a sample obtained through a mirror. As the X-ray tube, a plurality of optical fibers, according to claim in a bundle is used as a visible light guide unit for guiding visible light is formed around the X-ray guide portion for guiding the X-ray to the center 1 X-ray analyzer described in 1 . As the X-ray conduit, a hollow X-ray guide portion for guiding X-rays is formed at the center of a thick glass rod, a visible light guide portion for guiding visible light is formed around the X-ray conduit, and the glass The X-ray analyzer according to claim 1, wherein a material obtained by polishing both end faces of the rod is used .

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