JP2003028815A - X-ray analyzer and x-ray conduit used in the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an X-ray analyzer which can quickly and correctly confirm an X-ray irradiation position or an irradiation area at a sample and can efficiently measure, and an X-ray conduit used in the same. SOLUTION: In the X-ray analyzer which is constituted to irradiate X-rays (a) from an X-ray source 4 to the sample 2 by reducing X-rays, there are set between the X-ray source 4 and the sample 2, a visible light mirror 9 which passes the X-rays (a) and reflects a visible light e, and the X-ray conduit 10 where a visible light guide part 15 for passing the visible light e is formed to the periphery of an X-ray guide part 14 for guiding the X-rays (a). The irradiation position or the area of the X-rays (a) to the sample 2 can be confirmed on the basis of an optical image 24 of the sample obtained through the visible light guide part 15 and the visible light mirror 9 when the sample 2 is irradiated with a visible light d.

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 elements contained in a sample, their amounts and distribution states thereof, and an X-ray conduit used therefor.

[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 the fluorescent X-rays and transmitted X-rays generated at that time are detected by a detector. By appropriately processing the detection output, the constituent elements and internal structure of the sample are analyzed.

By the way, when performing measurement using the above-mentioned X-ray analysis apparatus, it is necessary to specify in advance a measurement point (a point to be irradiated with X-rays) in the sample before irradiating the sample with X-rays. Conventionally, as shown in FIG. 5, X-rays (primary X-rays) irradiated to a sample 52 placed on a sample table 51 are used.
The sample 52 is observed by an optical microscope or a CCD camera 54 from a direction different from the line 53 and the measurement point is indicated by a laser pointer (not shown), or a cross marker (not shown) is superposed on the obtained image. Was shown. In FIG. 5, 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 irradiation of the primary X-rays 53 on the sample 52, 59 is a lens, 6
Reference numeral 0 is a light guide for guiding visible light with which the sample 52 is irradiated.

[0004]

However, the above-mentioned conventional methods have the following disadvantages. That is, in order to make the sample 52 easier to find, if the lens 59 is of an exchangeable type or if a sume lens is used, the optical axis is displaced and the cost is increased.

In the above-mentioned conventional method, since the irradiation direction of the primary X-ray 53 to the sample 52 and the optical observation direction of the sample 52 are different, the sample 52 on the sample table 51 is different.
If the height of the X-ray changes, the irradiation position of X-rays in the optical image changes.

If the adjustment is insufficient, the exact X-ray irradiation position cannot be known. Further, even if the adjustment is accurately made at first, there is a disadvantage that it is hard to notice even if the irradiation position is displaced due to a disturbance such as a physical shock.

The present invention has been made in consideration of the above matters, and an object thereof is to enable quick and accurate confirmation of the X-ray irradiation position or irradiation region in a sample, and efficient measurement. It is to provide an X-ray analysis device and an X-ray conduit used therefor.

[0008]

In order to achieve the above object, the present invention provides an X-ray analyzer for irradiating a sample with X-rays from an X-ray source. In addition, a visible light mirror that allows X-rays to pass through but reflects visible light, and an X-ray conduit in which a visible light guide unit that allows visible light to pass through is provided around the X-ray guide unit that guides X-rays. The irradiation position or the irradiation region of the X-ray on the sample can be confirmed based on the optical image of the sample obtained through the visible light guide unit and the visible light mirror when the sample is irradiated with visible light (claim) Item 1).

According to the above X-ray analysis apparatus, it is possible to surely confirm the position or area irradiated with X-rays based on the optical image of the sample.

As the X-ray conduit used in the X-ray analyzer of the present invention, a plurality of optical fibers are provided at the center of the X-ray conduit.
X-rays are guided to the center of a thick glass rod or a bundle of visible light guides that guide visible light around the X-ray guide that guides the rays. A hollow X-ray guide portion is formed, a visible light guide portion for guiding visible light is formed around the hollow X-ray guide portion, and both end surfaces of the glass rod are polished (claim 3). You can

[0011]

DETAILED DESCRIPTION OF THE INVENTION The details of the present invention will be described below with reference to the drawings. FIG. 1 is a diagram schematically showing a configuration of a main part of an X-ray analysis apparatus according to the present invention. In FIG.
Is a horizontal sample stage for holding the sample 2, and a holding mechanism 3
It is configured to be linearly movable in the X direction (left and right direction of the paper surface), the Y direction (direction perpendicular to the paper surface), and the Z direction (vertical direction along the paper surface). Reference numeral 4 denotes an X-ray source provided above the sample stage 1, which comprises an appropriate X-ray tube or a mechanism for narrowing X-rays to a predetermined beam diameter (for example, a diameter of 100 μm), and an X-ray having a predetermined diameter (primary X-ray). a is emitted to the sample 2 on the sample stage 1.

Reference numeral 5 denotes a fluorescent X-ray detector which is, for example, a semiconductor detector for detecting fluorescent X-rays b generated in the sample 2 when the sample 2 on the sample stage 1 is irradiated with the primary X-ray a. It is provided at an appropriate position above the sample stage 1 at the tip of a housing 6 connected to a tank (not shown) containing a cooling medium. Reference numeral 7 is a transmission X-ray detector for detecting the transmission X-rays 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.

An illuminating device 8 appropriately illuminates the sample 2 on the sample stage 1 and comprises a light source which emits a visible ray d.

A visible light mirror 9 and an X-ray conduit 10 are serially provided in this order between the X-ray source 4 and the sample 2 on the sample stage 1. The visible light mirror 9
Is configured to pass X-rays but reflect visible rays. In this embodiment, a visible-light reflecting surface 11 is formed on one surface and, for example, 100 μm is formed in the center thereof.
The pinhole mirror is provided with a pinhole 12 capable of passing the X-ray a having a diameter of m. And
The visible light mirror 9 is interposed so that the visible light reflecting surface 11 faces the sample stage 1 side and forms an inclination angle of, for example, 45 ° with the irradiation direction of the X-ray a (irradiation optical axis 13).

The X-ray conduit 10 is provided around the central X-ray guide portion 14 for guiding the X-rays a and around the X-ray guide portion 14, and guides the visible light rays e from the sample 2. In this embodiment, as shown in an enlarged view in FIG. 3, a large number of optical fibers 16 are formed in a cylindrical sheath tube 17 made of an appropriate material and having an appropriate thickness. For example, one optical fiber 17 located at the center of the bundle is extracted, and the perforated part after the extraction is finished into a smooth surface (mirror surface state), and the X-ray guide unit 1
4 is set. Therefore, this X-ray conduit 10
Is a visible light guide unit 1 including a large number of optical fibers 16.
An X-ray guide portion 14 is provided at the center of 5 in the lengthwise direction, and is provided in the vertical direction so as to be parallel to the irradiation optical axis 13.
Further, both ends of the X-ray guide unit 14 and both ends of the visible light guide unit 15 including a large number of optical fibers 16 are aligned so as to be flush with each other.

The outer diameter of each 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. And
Such an X-ray conduit 10 has its X-ray guide portion 14
It is arranged so as to be concentric with the pinhole 12 of the visible light mirror 9. In addition, the plurality of optical fibers 16 are connected to the sheath tube 1
As a device housed in a bundle in 7, for example, a fiber optics plate (FO) manufactured by Hamamatsu Photonics KK
There is P).

In this embodiment, a small 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 visible light guide portion 15 has a small gap. Since the optical image is blurred, a condenser lens 18 such as a convex lens is provided in the gap to prevent the image from being blurred. FIG. 2 is an enlarged view of the 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 the X-ray a to pass through is provided in the center of the condenser lens 18 in the thickness direction thereof.

Referring again to FIG. 1, an optical image capturing unit 20 is provided on the reflection optical axis 21 (perpendicular to the irradiation optical axis 13) of the visible light mirror 9, and the sample 2 is irradiated with visible light by the illumination device 8. which captures an optical image of the sample 2 when illuminated by d, for example an optical microscope or CC
It consists of a D camera.

The reference numeral 22 controls the entire apparatus, the detector 5,
7 is an arithmetic and control unit for processing the output signal of 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, and includes a color display 23 as an output device and a keyboard or a mouse as an input device ( (Not shown).

The operation of the X-ray analyzer having the above structure will be described. Prior to irradiation of the sample 2 with the X-ray a, confirmation of the X-ray irradiation position or irradiation region of the sample 2 is performed as follows. That is, the X-ray source 4 emits X-ray a to the center of the sample 2 mounted on the sample stage 1, and the illumination device 8 emits visible light d. As a result, the X-ray a irradiates the sample 2 through the pinhole 12 of the visible light mirror 9 and the X-ray guide portion 14 of the X-ray conduit 10 and the X-ray guide hole 19 of the condenser lens 18. On the other hand, the visible light d from the illumination device 8 is the sample 1
Irradiate the entire surface.

The visible light e from the sample 2 whose entire surface is irradiated with the visible light d enters the visible light guide portion 15 through the condenser lens 18, and is further reflected by the visible light mirror 9.
Is reflected by and is captured by the optical image capturing unit 20,
Screen 23 of color display 23 of computer 22
On a, an optical image of the entire sample 2 as indicated by reference numeral 24 is displayed in a state of being magnified at a predetermined magnification. At this time,
An area indicated by reference numeral 25 is enlarged and displayed at the same magnification approximately at the center of the optical image 24. This region 25 shows the irradiation position of the X-ray a on the sample 2. That is, when the sample 2 is irradiated with the X-ray a and the visible light d at the same time, the irradiation position of the X-ray a is a portion (area) 25 which is omitted in the optical image 24 of the sample 2 by a predetermined size. Is displayed, it is possible to confirm the irradiation position or irradiation region of the X-ray a with respect to the sample 2 by visually confirming the position of the missing portion 25. After confirming the irradiation position or irradiation region, a predetermined X-ray analysis is performed.

The optical image 24 does not necessarily have to display the entire sample 2 and may be partially enlarged.

As described above, in the X-ray analyzer having the above structure, the irradiation position or area of the X-ray a with respect to the sample 2 can be surely confirmed based on the optical image 24 of the sample 2, and the X-ray a The irradiation position or the irradiation area of can be always surely grasped. Since no adjustment is required to confirm the irradiation position or irradiation region, the confirmation work can be performed extremely easily.

In the above embodiment, the condenser lens 18 is provided 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 being blurred. ,
The gap between the lower end surface of the X-ray conduit 10 and the sample 2 is 1 m.
When they are brought close to each other so that the distance becomes m or less, the installation of the condenser lens 18 can be omitted. It is preferable that the lower end surface of the X-ray conduit 10 and the sample 2 are 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.

The present invention is not limited to the above-described embodiment, but the X-ray conduit 10 shown in FIG. 4 may be used. That is, in this figure, 26 is 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 longitudinal direction. The portion 28 is finished smoothly (to a mirror surface state) to form an X-ray guide portion, and the periphery of the X-ray guide portion 28 is formed as a guide portion 29 that allows visible rays to pass therethrough. In addition, this glass rod 27
Both end surfaces 27a, 27b in the length direction of the are polished and finished so as to be mirror-finished.

The visible light mirror 9 is not limited to the pinhole mirror, and may be formed of, for example, Be (beryllium), which has a property of passing X-rays but not visible light through the mirror body. Good.

[0027]

According to the X-ray analysis apparatus of the present invention, the position or area irradiated with X-rays can be surely confirmed on the basis of the optical image of the sample, and no further adjustment is necessary for the confirmation. Since it is not necessary, the confirmation work can be performed extremely easily and quickly.

The X-ray conduit of the present invention has a simple structure, is easy to handle, and is easy to manufacture. Therefore, it can be suitably used as an X-ray guide member in an X-ray analyzer. .

[Brief description of drawings]

FIG. 1 is a diagram schematically showing a configuration of a main part of an X-ray analysis apparatus of 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 analysis apparatus.

FIG. 3 is an enlarged perspective view showing an example of an X-ray conduit incorporated in the X-ray analysis apparatus.

FIG. 4 is an enlarged perspective view showing another example of the X-ray conduit.

FIG. 5 is an explanatory diagram of a conventional technique.

[Explanation of symbols]

2 ... Sample, 4 ... X-ray source, 9 ... Visible light mirror, 10 ... X-ray conduit, 14 ... X-ray guide section, 16 ... Visible light guide section, 1
7 ... Optical fiber, 24 ... Optical image of sample, 26 ... X-ray conduit, 27 ... Glass rod, 27a, 27b ... End surface, 28
... X-ray guide section, 29 ... Visible light guide section, a ... X-ray, d
... visible light, e ... visible light.

Continued front page    F-term (reference) 2G001 AA01 AA07 BA04 BA11 CA01                       DA01 DA02 DA06 GA04 HA13                       KA01 SA01 SA02 SA04

Claims (3)

[Claims] 1. An X-ray analyzer adapted to irradiate a sample with X-rays from an X-ray source. Visible light that allows X-rays to pass through but reflects visible light between the X-ray source and the sample. A mirror and an X-ray conduit in which a visible light guide portion that allows visible light to pass therethrough is formed around the X-ray guide portion that guides X-rays, and the visible light guide portion when the sample is irradiated with visible light. And an X-ray irradiation position or irradiation area on the sample can be confirmed based on an optical image of the sample obtained through the visible light mirror.
Line analyzer. 2. An X-ray conduit characterized in that a plurality of optical fibers are bundled so that a visible light guide unit for guiding visible light is formed around an X-ray guide unit for guiding X-rays in a central portion. . 3. A hollow X-ray guide portion for guiding X-rays is formed at the center of a thick glass rod, and a visible light guide portion for guiding visible light is formed around the hollow X-ray guide portion. An X-ray conduit characterized in that both end faces of the are polished.