JP3465136B2 - Cylindrical crystal spectrometer and X-ray analyzer using the same - Google Patents

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a cylindrical crystal type spectroscopic device and an X-ray analysis device using the same.

[0002]

2. Description of the Related Art Conventionally, in the case of analyzing a sample with an X-ray analyzer, a radiant X-ray generated by an X-ray tube is applied to a sample on a sample table, and a fluorescent X-ray generated from this sample is used. The next X-ray is detected by the detector. Here, a spectroscopic element composed of a curved crystal is arranged between the X-ray tube and the sample, and thereby the emitted X-ray is diffracted into a monochromatic light, which has a wavelength of 1 required for analysis of a specific element to be analyzed in the sample. The next X-ray is generated and this primary X
By irradiating a sample with a line, the analysis accuracy of a specific element is improved. Further, it is also possible to analyze a trace element by disposing a collimator or a capillary between the X-ray tube and the sample, focusing the X-ray with these and irradiating the sample with the X-ray having high intensity. There is.

However, since the above collimators and capillaries do not have a spectroscopic function, the emitted X-rays cannot be monochromatic, and the analysis accuracy of specific elements cannot be improved. Further, when the dispersive element made of a curved crystal is used, the radiant X-ray can be monochromatic, but the dispersive element as a whole becomes large. Therefore, the applicant of the present application, in the above-mentioned Japanese Patent Application No. 9-183751, uses a cylindrical spectroscopic element, and
We proposed a device that monochromaticizes the next X-ray and irradiates the sample.

[0004]

In the technique of this prior application,
Since the monochromatic primary X-rays are point-focused and irradiated on a small area on the sample with high intensity, the analysis accuracy of the sample is improved. However, depending on the sample, it may be desired to irradiate a large area with the primary X-ray. For example, when analyzing alloys or ores in which the contained elements are easily segregated, in order to reduce the influence of segregation, a large area of the sample is usually irradiated with X-rays and the average of various elements contained in the sample is averaged. Perform compositional analysis. The device of the prior application cannot be used as it is for a sample having such a wide analysis area.

The present invention makes it possible to perform high-accuracy analysis by irradiating a relatively small area of a sample with high-intensity primary X-rays while reducing the size of the entire spectroscopic element, and radiating X-rays to a relatively large area of the sample. A cylindrical crystal type spectroscopic device and a cylindrical crystal type spectroscopic device that can be used to significantly expand the application It is an object of the present invention to provide an X-ray analysis device that has been used.

[0006]

In order to achieve the above object, a cylindrical crystal type spectroscopic device according to a first aspect of the present invention comprises a cylindrical spectroscopic element that disperses X-rays, and A first slit member having an annular slit for passing X-rays incident on the peripheral surface, and a second slit member having an annular slit for passing X-rays emitted from the inner peripheral surface of the spectroscopic element, Each of the first and second slit members has a central passage hole through which X-rays pass at the center thereof, and X-rays are selectively emitted through the central passage hole and the annular slit. A switching shutter for opening and closing the line passage is provided.

According to the first aspect of the invention described above, high-precision analysis of a sample with a primary X-ray using a spectroscopic element by a shutter switching operation on a relatively narrow irradiation surface and sample with radiant X-ray without a spectroscopic element. It is possible to selectively perform an average composition analysis on a relatively wide irradiation surface of. That is, by opening the primary X-ray passage that passes through the annular slits of the first and second slit members by operating the shutter, the radiation X-rays from the X-ray tube are narrowed down by the annular slit of the first slit member. , Is incident on the inner peripheral surface of the cylindrical spectroscopic element while drawing an inverted conical incident optical path. Then, the radiated X-rays are separated (monochromaticized) on the inner peripheral surface, and the primary X-rays necessary for the analysis of the measurement target element contained in the sample are extracted. Further, the primary X-ray is emitted from the inner peripheral surface at the same angle as the incident angle, narrowed down by an annular slit provided in the second slit member, and has a conical emission optical path opposite to that at the time of incidence. The light is emitted outward while drawing and is irradiated on a small irradiation surface on the measurement surface of the sample, and high-precision analysis of the sample is performed.

Further, by opening the radiant X-ray passage passing through the central passage hole of each slit member by operating the shutter, the radiant X-rays from the X-ray tube pass through the respective central passage holes and reach a wide irradiation surface of the sample. The composition is directly irradiated and the average composition of various elements contained in the sample is analyzed.

As described above, when the shutter is switched,
By selectively performing the high-precision analysis of the sample by the primary X-ray that has passed through the spectroscopic element and the average composition analysis of the sample by the radiant X-ray, the average analysis of the alloy or ore in which the elements are easily segregated can be performed. Can be supported, and the application will be expanded significantly. Moreover, when performing high-precision analysis of the sample, the shutter opens the annular slits of each slit member, and the X-rays are incident and emitted while these slits are narrowed. By reflecting the primary X-rays over the entire surface, a large amount of the primary X-rays can be concentrated on the sample, and the trace elements can be analyzed satisfactorily. Further, since the sample is irradiated with the primary X-ray after being monochromatic by the spectroscopic element, the analysis accuracy of the specific element can be improved. Moreover, by making the spectroscopic element cylindrical, the entire element becomes smaller.

According to a second aspect of the present invention, there is provided a cylindrical crystal type spectroscopic device, wherein a cylindrical spectroscopic element that disperses X-rays and an annular slit that allows X-rays incident on the inner peripheral surface of the spectroscopic element to pass therethrough. And a second slit member having an annular slit that allows X-rays emitted from the inner peripheral surface of the spectroscopic element to pass therethrough. These first and second slit members are provided at the center. An opening / closing shutter which has a central passage hole for passing X-rays, and further selects an open state in which the X-rays passing through the central passage hole are allowed to enter the sample and a closed state in which the X-rays are blocked. I have it.

According to the above second invention, the same operation as that of the first invention can be obtained. That is, when performing high-precision analysis of the sample, the radiation X-ray passage that passes through the central passage holes of the first and second slit members is closed by operating the opening / closing shutter. And
Radiated X-rays from the X-ray tube are made incident on the spectroscopic element from the first slit member, and primary X-rays reflected therefrom are emitted from the second slit member onto a small area of the sample. Further, when performing an average composition analysis in a wide area of the sample, the radiation X-ray passage is opened by operating the shutter. As a result, in addition to the primary X-rays that have passed through the spectroscopic element, the emitted X-rays are directly irradiated over a wide area of the sample.

The spectroscopic element is housed and held in a holder,
Further, it is preferable that a shutter case is attached to the holder, and the opening / closing shutter is rotatably supported therein (claim 3).

An X-ray analysis apparatus according to a third aspect of the present invention is a sample stage that supports a sample and an X-ray that irradiates the sample.
An X-ray tube that generates X-rays, a cylindrical spectroscopic element that disperses X-rays, and an annular slit that allows passage of X-rays that are generated from the X-ray tube and incident on the inner peripheral surface of the spectroscopic element 1
A slit member, a second slit member having an annular slit for passing X-rays emitted from the inner peripheral surface of the spectroscopic element, a sample stage, or an X-ray tube, a spectroscopic element, and first and second
And a moving device that moves at least one of the set with the slit member in the axial direction of the spectroscopic element with respect to the other.

According to the above X-ray analysis apparatus, as in the case of each invention, the radiation X-rays from the X-ray tube are incident on the spectroscopic element from the first slit member, and the primary X-rays are the second slit member. The sample held on the sample table is irradiated with the light. At this time, one of the sample stage side and the X-ray tube side (including the spectroscopic element and the first and second slit members) is moved by the moving device in the axial direction of the spectroscopic element with respect to the other, and the two are moved between them. The relative position between the focal point of the primary X-ray emitted from the second slit member and the sample is changed by changing the distance. Therefore, by changing the distance between the two with the moving device and shifting the focal point of the primary X-ray from the sample, the primary X-ray is irradiated onto a wide area of the sample, and the average composition analysis of this sample is performed. Also, 1
By making the sample close or coincide with the focal point of the next X-ray, the primary X-ray is point-focused on the sample, and high-precision analysis of this sample is performed.

[0015]

BEST MODE FOR CARRYING OUT THE INVENTION An embodiment of the present invention will be described below with reference to the drawings. FIG. 1 schematically shows an X-ray analyzer. In this device, an X-ray tube 1 containing an X-ray source G
, And the cylindrical crystal type spectrometer 2 is attached to the upper part. Then, the radiant X-rays emitted from the X-ray tube 1 are dispersed by the spectroscopic device 2 to extract the primary X-rays b necessary for the analysis of the specific element, and the primary X-rays b are formed in the sample stage 3 to form an opening. From 30, the measurement surface of the sample 4 held on it is irradiated, and the secondary X-rays c such as fluorescent X-rays generated from this sample 4 are detected by the detector 5.

As shown in FIG. 2, the X-ray tube 1 causes the electron beam d generated by the filament 7 provided in the casing 6 to collide with the target 8, and the radiant X-ray a generated at this time is emitted from the casing 6. The light is emitted toward the spectroscopic device 2 from a window material 9 such as a beryllium film provided on the upper side.

The cylindrical crystal type spectroscopic device 2 used in the above X-ray analyzer comprises a cylindrical spectroscopic element 10 and a plurality of divided pieces 11a divided in the circumferential direction, and supports the outer peripheral surface of the spectroscopic element 10. Cylindrical crystal stand 11 and crystal stand 11 on the inner circumference
Is provided with a cylindrical holder 12 having a joining surface 12a to which is joined. Then, the crystal stage 11 is mounted inside the holder 12, and the spectroscopic element 10 is mounted concentrically on the inner surface thereof. Further, the holder 12 has a disc-shaped first slit member 13 on the lower side which is the incident side of the primary X-rays b, and a disc-shaped second slit member 14 on the upper side which is the emission side. It is fixed by a plurality of mounting screws 15. The slit members 13 and 14 have annular slits 13a,
14a, and central passage holes 13b and 14b are formed in the central portions thereof to form slits 13
An X-ray passage passing through a and 14a and the central passage holes 13b and 14b is selectively opened and closed by a switching shutter 40 described later.

[0018] The spectroscopic element 10 songs Gaité form tabular material into a cylindrical shape such as lithium fluoride and mica. In this way, the cylindrical spectroscopic element 10 can be easily manufactured, and the spectroscopic element 10 can be downsized.

Each of the slit members 13 and 14 is, for example, as shown in FIG. 3, a thin metal flat plate 16 is used, a plurality of circumferential positions are left as connecting portions 16a, and the slit members 13 and 14 are peeled off in an arc shape by an etching means or the like. By pulling out, connecting part 1
The continuous annular slits 13a and 14a are formed through 6a. At the same time, central passage holes 13b and 14b are formed in the circular arc centers of the annular slits 13a and 14a.

The peripheral wall 12b of the holder 12 shown in FIG.
An injection hole 12c penetrating the peripheral wall 12b in the radial direction is formed, and an adhesive 17 is injected into the joint surface 12a on the inner circumference from the outside, and the crystal stage 11 fitted to the holder 12 by the adhesive 17 is formed. The divided pieces 11a are integrally joined to the joint surface 12a.

Further, the peripheral wall 12b is provided on the peripheral wall 12b.
A plurality of adjusting screw bodies 18 that pass through b in the radial direction are screwed together, and the tips of the adjusting screw bodies 18 abut on the outer peripheral surfaces of the divided pieces 11a of the crystal base 11 to regulate the radial positions of these divided pieces 11a. ing.

The holder 12 is fixed to the X-ray tube 1 by screwing a plurality of fixing screws 19 from the flange portion 12d provided on the lower side thereof to the flange portion 1a provided on the upper side of the X-ray tube 1. In contrast, it is detachably attached.

Further, the flange portion 12d of the holder 12
A plurality of height adjusting screws 20 are provided on the
The height of the spectroscopic device 2 with respect to the X-ray tube 1 is finely adjusted by rotating each adjusting screw 20 in a state where the adjusting screw 20 is in contact with the upper end surface of the flange portion 1a provided in the X-ray tube 1. There is.

A conical cylindrical cap 21 is provided on the upper side of the holder 12 where the primary X-rays b are emitted. The cap 21 is fastened together with the second slit member 14 to the upper end of the holder 12 by a mounting screw 15.

Further, as shown in FIG. 4, the annular slits 13a, 1 are provided on the exit side of the second slit member 14.
4a and the central passage holes 13b and 14b are selected, and a switching shutter 4 for passing either the primary X-ray b or the radiant X-ray a
0 is arranged outside the spectroscopic device 2. Specifically, a column 41 is mounted on the X-ray tube 1 on the side of the spectroscopic device 2, and a slider device 43 having a motor 42 as a power source is attached to the column 41. The support rod 44 extending from 40 is slid to perform the switching operation of the switching shutter 40a. The control of the motor 42a is performed by a controller (not shown) that operates by receiving a manual instruction. As described above, when the switching shutter 40 is provided on the emission side of the second slit member 14 and outside the spectroscopic device 2, it is not necessary to change the optical system of the spectroscopic device 2. It can be installed easily. The support column 41 may be attached to the holder 12 of the spectroscopic device 2.

As shown in FIG. 5, the shutter 40 has annular slits 13a, 1 of the slit members 13, 14 respectively.
An annular switching slit 45 for passing a primary X-ray b passing through 4a and a pinhole 46 for passing a radiant X-ray a passing through each of the central passage holes 13b and 14b are formed separately in the sliding direction X. Has been done. The switching slit 45 is formed in the same manner as in the case of FIG. 3, but it does not narrow down the X-ray but merely allows it to pass through, so the opening may be set slightly larger. Further, a plurality of pinholes 46 having different diameters are provided in the shutter 40, and arbitrary pinholes are selected according to the analysis application, and the irradiation amount of the radiant X-ray a to the sample 4 by these pinholes is changed. You may be allowed to.

Next, the operation of the above configuration will be described. When performing high-precision analysis of the sample 4 using the spectroscopic element 10, as shown in FIG. 6, the shutter 40 is moved via the slider device 43 by driving the motor 42,
The switching slit 45 is provided for each of the slit members 13,
The annular slits 13a and 14a of 14 are concentrically opposed to each other, and the passage of the primary X-ray b passing therethrough is opened.
Then, the radiated X-ray a from the X-ray tube 1 is narrowed down by the annular slit 13 a of the first slit member 13, and enters the inner peripheral surface of the spectroscopic element 10 while drawing an incident light path having an inverted conical shape. Then, the radiated X-ray a is diffracted on this inner peripheral surface according to the Bragg's equation to be monochromatic, and the primary X-ray b necessary for the analysis of the element to be measured contained in the sample 4 is generated.

The primary X-ray b is emitted at the same angle as the incident angle on the inner peripheral surface, is narrowed down by the annular slit 14a of the second slit member 14, and is emitted in a conical shape opposite to that at the time of incidence. While drawing the incident light path, it is emitted to the sample 4 side through the slit 45 of the shutter 40, and this emitted light path forms a focal point f at a point on the measurement surface of the sample 4. That is, the high-intensity primary X-rays b monochromaticized by the spectroscopic element 10 having a wide cylindrical spectral surface is intensively applied to one point on the sample 4. Secondary X-rays c such as fluorescent X-rays generated from the sample 4 are incident on the detector 5 by the irradiation of the strong primary X-rays b, and highly sensitive analysis of trace elements contained in the sample 4 is performed. Be seen. In addition, since the sample 4 is irradiated with the primary X-rays b monochromaticized by the spectroscopic element 10, the analysis accuracy of the specific element is also improved.

At this time, by rotating each of the adjusting screws 20 shown in FIG. 2 to finely adjust the height of the spectroscopic device 2 with respect to the X-ray tube 1, the light emitted from the spectroscopic device 2 1
The focus f of the next X-ray b is adjusted to one point on the measurement surface of the sample 4. In this case, the shutter 40 blocks the passage of the radiant X-ray a that reaches the sample 4 through the central passage holes 13b and 14b of the slit members 13 and 14, respectively.

On the other hand, when performing an average composition analysis of a wide area of the sample 4 by the radiant X-ray a without using the spectroscopic element 10, as shown in FIG. 7, the switching shutter is used by the slider device 43. 40 is moved so that the pinhole 46 is positioned to face the central passage holes 13b and 14b of the slit members 13 and 14, respectively. Then, the primary X that reaches the sample 4 through the annular slits 13a and 14a.
The passage of the line b is blocked, and the emitted X-ray a from the X-ray tube 1 is
The sample 4 is directly irradiated from the passage holes 13b and 14b through the pinhole 46, and the sample 4 is analyzed. At this time, the radiant X-ray a is not focused into a conical shape as in the case of using the spectroscopic element 10, and directly passes through the passage holes 13b and 14b through the pinholes 46 over a relatively wide irradiation surface of the sample 4. Is irradiated. Therefore, as compared with the case where the spectroscopic element 10 is used, the background component is large and it is not suitable for highly accurate analysis, but the X-ray intensity is high because it is not monochromatic, so that the wide irradiation surface of the sample 4 is used. The rough composition analysis is performed, and the average analysis of various elements contained in the sample 4 becomes possible.

As described above, if the high-precision analysis in the narrow region of the sample 4 and the average composition analysis in the wide region can be selectively performed, the use of the spectroscopic device 2 is greatly expanded. It That is, for example, when analyzing a wiring pattern of a printed circuit board, the spectroscopic element 10 is used to perform a local highly accurate analysis of the wiring pattern and the like. Further, for example, when analyzing various compositions contained in a coating film, earth and sand, a metal block, etc., the spectroscopic element 10 is used.
An average composition analysis is performed on a wide portion of the composition by the radiant X-ray a without using. Further, in the case of analyzing foreign matter such as dirt attached to the sample, first, without using the spectroscopic element 10, the entire sample is roughly analyzed by the radiant X-ray a to find a portion where the foreign matter exists, and then, The spectroscopic element 10 is used to intensively irradiate monochromatic primary X-rays b to the narrowly spotted area that has been found, and the foreign matter is precisely analyzed.

Further, as described above, the spectroscopic element 10, the crystal stage 11 and the holder 12 shown in FIG. 2 are each formed in a cylindrical shape, and these members are arranged concentrically, thereby making it possible to downsize the entire apparatus. Become.

Moreover, since the above-described spectroscopic device 2 is detachably attached to the X-ray tube 1 through the plurality of fixing screws 19, the spectroscopic element having different crystal plane intervals and the annular slit having different diameters are provided. Various spectroscopic devices 2 are selected, and sample 4
By replacing the X-ray tube 1 that emits a primary X-ray having an optimum wavelength for the analysis of a specific element contained in
Highly accurate analysis of the sample 4 can be performed.

In the above embodiment, the shutter 40 is arranged on the exit side of the second slit member 14, but the shutter 40 may be arranged on the entrance side of the first slit member 13. In that case, the switching shutter 40 is fixed with the fixing screw 19.
And, it is inserted into the X-ray passage from between the adjusting screw 20. Further, the shutter 40 may be manually switched without using the motor 42.

FIG. 8 shows a cylindrical crystal type spectroscopic device 2 of another embodiment. In this spectroscopic device 2, a shutter case 22 is attached to an upper portion of a holder 12 in which the spectroscopic element 10 and the first and second slit members 13 and 14 are incorporated, and inside the shutter case 22, each of the slit members 13,
Radiant X-ray a that has passed through 14 central passage holes 13b and 14b
The open / close shutter 50 is rotatably supported to select an open state that allows the light to enter the sample 4 and a closed state that blocks the radiation X-ray a.

As shown in FIG. 9, the opening / closing shutter 50 uses a prismatic shutter main body 51 having six first to sixth surfaces 51a to 51f, and the first and fourth shutter bodies 51 facing each other are provided.
First and second insertion holes 52 and 53 are formed between the surfaces 51a and 51d and the second and fifth surfaces 51b and 51e, respectively, to allow the radiation X-ray a to enter the sample side. Also,
The third and sixth surfaces 51c and 51f are closed surfaces 54. Further, on the fifth surface 51e on one end side of the second through hole 53,
As shown in FIG. 10, for example, a filter 55 for reducing the X-ray intensity on the low energy side is attached (see FIG. 11 described later).

On both sides of the shutter body 51,
The two support shafts 56 and 57 shown in FIG. 9 are mounted concentrically,
These are inserted into the wall portion of the shutter case 22 of FIG. 8, and the shutter main body 51 is rotatably supported therein. Furthermore, when the shutter body 51 is attached to the shutter case 22, an operation groove 58a for rotating the shutter body 51 is formed at an end portion of the support shaft 57 when the shutter body 51 is attached to the shutter case 22. A circular operation unit 58 is provided. Further, a pressing spring 23 having a protrusion 23a for nodal movement is attached to the shutter case 22 with a screw body 24, and the protrusion 23a is locked in a recessed portion provided in the operation portion 58,
Positioning of the shutter body 51 in the rotational direction is performed.

Then, a tool is inserted into the operation groove 58a of the operation portion 58 from the outside to rotate the shutter main body 51, and the first through hole 52 is positioned so as to face the central passage holes 13b and 14b. Radiant X-ray a from 1
Is directly irradiated onto the sample 4 through each hole, and an average composition is analyzed in a wide region (analysis area) of the sample 4.
Further, by arranging the second through hole 53 shown in FIG. 10 to face the central passage holes 13b and 14b of FIG. 8, the radiant X-ray a is applied to the sample 4 through the filter 55 (FIG. 10),
Analysis of the sample 4 with the radiation X-ray a that has passed through the filter 55 is performed in a relatively low background. At this time, part of the radiant X-ray a shown in FIG. 8 enters the spectroscopic element 10 through the slit 13a of the first slit member 13,
The primary X-ray b thus generated is applied to the sample 4 from the slit 14a of the second slit member 14.

Further, by arranging the closing surface 54 of FIG. 10 to face the central passage holes 13b and 14b of FIG. 8, the radiation X-ray a is blocked. Then, only the primary X-ray b which has passed through the slit 13a of the first slit member 13 and which has been monochromatized by the spectroscopic element 10 is irradiated to the sample 4 from the slit 14a of the second slit member 14, and the sample 4 High-precision analysis with low background is performed.

In FIG. 11, the vertical axis represents the intensity of X-rays (dimensionless),
The X-ray spectrum obtained by the spectroscopic device 2 with energy taken on the horizontal axis is shown. In the figure, a curve A indicated by a solid line is a dotted line indicating the intensity when the sample 4 is directly irradiated with the radiant X-rays a that are continuous X-rays from the first through hole 52 without using the spectroscopic element 10. The curve B shown is the radiant X-ray a
Through the filter 55 provided in the second through hole 53
And the curve C shows the intensity when the sample 4 is irradiated with only the primary X-ray b which is monochromatic and which blocks the radiant X-ray a. The figure shows
Molybdenum (Mo) is used as the anode metal and the voltage is 30
The X-ray intensity when KV is applied is shown, and the maximum peak of the curve A shows the intensity of the Mo-Kα line.

By using continuous X-ray A, 5 to 3
Light elements to heavy elements can be excited over a wide range of 0 KeV, and by using filtered X-ray B, background components near 5 to 15 KeV are suppressed and the detection accuracy of elements near this is improved. Then, by using the monochromatic X-ray C, a light element having an energy slightly lower than the peak can be detected with high accuracy under a low background. As described above, by selecting various X-rays A to C by operating the opening / closing shutter 50 and irradiating the sample 4, a wide range from light elements to heavy elements contained in the sample 4 and a narrow range are measured. Highly accurate measurement in the range is possible.

The X-ray analysis apparatus shown in FIG. 12 has an X-ray tube 1 and a cylindrical crystal type spectroscopic apparatus 2 combined therewith,
The sample table 3 is supported by a moving device 60 so as to be movable in the axial direction of the spectroscopic element 10. As the moving device 60, in the embodiment shown in the figure, a screw rod 61 fixed to the X-ray tube 1 and extending vertically, a guide rod 62 parallel to the screw rod 61, and a motor 63 attached to the X-ray tube 1 are used. A worm gear 64 rotatably driven by the motor 63 is engaged with a gear portion 61a provided on the screw rod 61, and the sample table 3 is slidably connected to a screw portion 61b of the screw rod 61 via a ball screw 65. Further, the sample table 3 is supported by the guide rod 62 via a linear bearing 30 provided at one end thereof so as to be movable in the axial direction. The worm 64 is rotated by the driving of the motor 63, and thereby the screw rod 61 is rotated, so that the sample stage 3 is moved along the screw rod 61 and the X-ray tube 1
And move vertically with respect to the spectroscopic device 2.

A detector 5 for detecting the secondary X-ray c generated from the sample 4 held on the sample table 3 is provided on the sample table 3.
It is attached via a mounting bracket 66. By doing so, the detector 5 moves following the sample table 3,
Good detection of the secondary X-ray c is possible. The detector 5
If the cylindrical body 5a for limiting the field of view provided in is shortened, the field of view becomes wider. Therefore, when the movement amount of the sample table 3 is small, the detector 5 does not necessarily need to be moved following the sample table 3.
For example, it can be fixed to the X-ray tube 1 so as to be immobile.

The X-ray analyzer of FIG. 13 uses an elevator lift 60A as the moving device, and mounts the X-ray tube 1 with the spectroscopic device 2 mounted on the elevator lift 60A attached to the base 69, This can be moved up and down with respect to the sample table 3 supported by the base 69. The lifting lift 60A
Includes a support base 70 that supports the X-ray tube 1 side, and a base 71 supported by a base 69. The support base 70 is rotatably connected to the lower side of the support base 70 in a central portion so as to be rotatable. Two links 72, 73, and two similar links 74, 75 on the upper side of the ground member 66 are pivotally supported respectively,
The lower ends of the upper links 72, 73 and the lower links 74,
The upper end of 75 is connected by connecting shafts 77 and 78. Further, each of the links 72 to 75 is arranged between the support base 70 and the base 71 in two sets at a predetermined interval in the front and back direction of the paper surface of FIG. 13, and the connected link ends are connected in the front and back directions. The connecting shafts 81 and 82 are connected to each other by connecting members 83 and 84, and the tip end of the screw shaft 87 having the operating portion 86 at the base end is rotatably connected to one connecting member 84. The threaded portion 87a of the portion is screwed to the other connecting member 83. Then, by rotating the screw shaft 87, each connecting shaft 8
By changing the relative distance between 1 and 82, the X-ray tube 1 side is moved up and down with respect to the sample table 3 via the support table 70.

Next, the operation of FIGS. 12 and 13 will be described. First, in the case of performing high-precision analysis of the sample 4, the X-ray tube 1 side or the sample table 3 is moved vertically with respect to the other side by the moving devices 60 and 60A, as shown in FIG. The radiation X-ray a emitted from the X-ray tube 1 and narrowed down by the first slit member 13 is made incident on the spectroscopic element 10, and the primary X-ray b monochromaticized by the spectroscopic element 10.
Is squeezed by the second slit member 14 to irradiate so that the focal point f is formed at one point on the measurement surface of the sample 4. This enables highly sensitive analysis of trace elements contained in the sample 4 with strong primary X-rays b, and also improves analysis accuracy of specific elements.

Next, when performing composition analysis on a wide analysis area of the sample 4, as shown in FIG. 15, the moving device 60 (see FIG. 15) is arranged so that the primary X-ray b is focused on the position below the sample 4. 12) and 60A (FIG. 13), the X-ray tube 1 side or the sample stage 3 is moved with respect to the other side. Then,
Since the focal point f is displaced from the analysis surface of the sample 4 and the primary X-rays b are irradiated over a wide area on the measurement surface of the sample 4, it is possible to measure the elements contained in this wide region on average. . Therefore, it is suitable for analyzing alloys and ores whose contained elements are easily segregated. Even if the focal point f of the primary X-ray b is shifted with respect to the measurement surface of the sample 4, the primary X-ray b
Since the total intensity of the line b is almost unchanged, good measurement of various elements can be performed. The focal point f of the primary X-ray b may be shifted to either the upper side or the lower side with respect to the measurement surface of the sample 4.

[0047]

As described above, according to the present invention, it is possible to perform a high-precision analysis by irradiating a relatively small area of a sample with a high-intensity primary X-ray, while reducing the size of the entire spectroscopic element. X
An average composition analysis can be performed by irradiating a relatively large area of a sample with a line, and this average composition analysis and high-precision analysis can be selected and performed, and elements are easily segregated. It can be used for analysis of alloys and ores, etc., and its applications can be greatly expanded.

[Brief description of drawings]

FIG. 1 is a side view schematically showing an X-ray analysis apparatus.

FIG. 2 is a vertical cross-sectional view showing a main part of a cylindrical crystal type spectroscopic device according to an embodiment of the present invention.

FIG. 3 is a plan view of each slit member used in the apparatus.

FIG. 4 is a side view showing the entire apparatus.

FIG. 5 is a plan view of a switching shutter used in the spectroscopic device.

FIG. 6 is a side view showing a method of using the same.

FIG. 7 is a side view showing another usage method.

FIG. 8 is a vertical cross-sectional view showing a cylindrical crystal type spectroscopic device according to another embodiment of the present invention.

FIG. 9 is a perspective view of an opening / closing shutter used in the apparatus.

FIG. 10 is a vertical sectional view of the shutter.

FIG. 11 is an X-ray spectrum diagram obtained by the same device.

FIG. 12 is a side view schematically showing an X-ray analysis apparatus according to an embodiment of the present invention.

FIG. 13 is a side view showing another embodiment of the X-ray analysis apparatus.

FIG. 14 is a side view showing the method of use.

FIG. 15 is a side view showing another usage method.

[Explanation of symbols]

1 ... X-ray tube, 3 ... sample stage, 4 ... sample, 10 ... spectroscopic element,
12 ... Holder, 13 ... 1st slit member, 14 ... 2nd slit member, 13a, 14a ... Slit, 13b, 14
b ... central passage hole, 22 ... shutter case, 40 ... switching shutter, 50 ... opening / closing shutter, 60, 60A ... moving device.

─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Yukio Sako 14-8 Akaoji-machi, Takatsuki City, Osaka Prefecture Rigaku Denki Kogyo Co., Ltd. (56) Reference JP-A-11-52096 (JP, A) JP Hei 10-300893 (JP, A) JP 61-88200 (JP, A) JP 11-14570 (JP, A) (58) Fields investigated (Int.Cl. ⁷ , DB name) G21K 1 / 06 G01N 23/223

Claims (4)

(57) [Claims] 1. A cylindrical spectroscopic element that disperses X-rays, a first slit member having an annular slit that allows X-rays incident on the inner peripheral surface of the spectroscopic element to pass therethrough, and an inner peripheral surface of the spectroscopic element. A second slit member having an annular slit that allows passage of X-rays emitted from the first and second slit members, the first and second slit members having a central passage hole that allows passage of X-rays in the center, and further, X A cylindrical crystal type spectroscopic device comprising a switching shutter that opens and closes an X-ray passage so that a ray selectively passes through the central passage hole and the annular slit and is emitted. 2. A cylindrical spectroscopic element that disperses X-rays, a first slit member having an annular slit that allows X-rays incident on the inner peripheral surface of the spectroscopic element to pass therethrough, and an inner peripheral surface of the spectroscopic element. A second slit member having an annular slit that allows passage of X-rays emitted from the first slit member, the first and second slit members having a central passage hole that allows passage of X-rays in a central portion, and further, A cylindrical crystal-type spectroscopic device having an open / close shutter that selects an open state that allows X-rays that have passed through the central passage hole to enter the sample and a closed state that blocks the X-rays. 3. The cylindrical crystal type spectroscopic device according to claim 2, further comprising a holder that holds the spectroscopic element, and a shutter case that rotatably supports the open / close shutter is attached to the holder. 4. A sample stage for supporting a sample, an X-ray tube for generating X-rays irradiated on the sample, a cylindrical spectroscopic element for separating X-rays, and the spectroscopic light generated from the X-ray tube. A first slit member having an annular slit that allows an X-ray incident on the inner peripheral surface of the element to pass therethrough; and a second slit member having an annular slit that allows an X-ray emitted from the inner peripheral surface of the spectroscopic element to pass therethrough. , A sample stage or an X-ray tube and a moving device for moving at least one of the set of the spectroscopic element and the first and second slit members in the axial direction of the spectroscopic element with respect to the other.
Line analyzer.