JPH0812157B2 - X-ray diffractometer - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial field of application] The present invention absorbs and stores radiation, and when stimulated by irradiation with excitation light, stimulated emission (once emission) Then, the X-ray diffraction image of the crystalline sample is accumulated and read on an image accumulating plate having a phosphor layer that erases the accumulated radiation image and returns to the original state. The present invention relates to a novel X-ray diffractometer for obtaining crystal structure information of a sample.

[Prior Art] An X-ray diffraction apparatus for obtaining crystal information of a sample by recording an X-ray diffraction image obtained when a crystalline sample is irradiated with monochromatic X-rays on a certain recording medium and reading it. Conventionally, for example, a device based on a camera method such as a Laue camera, a Debye-Scherrer camera, or a cylindrical camera has been known (for example, Seiko Tanaka et al. “Instrument Analysis” published by Sokabo.
(Refer to 152) [Problems to be solved by the invention] However, in the measurement by these camera methods, usually, after setting the film on the camera and exposing it by X-ray, the film is removed from the camera, and then development and printing are performed. It has a drawback that the measurement work is complicated and the measurement requires a long time.

In particular, in the case of the above-mentioned cylindrical camera method, it is necessary to cut the film into a predetermined shape, form it into a cylindrical shape, and set it in the cylinder of the cylindrical camera, and also to perform processing such as development and printing. It was extremely complicated.

The object of the present invention is to provide a new X-ray diffractometer in which the above-mentioned drawbacks have been eliminated.

[Means for Solving the Problems] The present invention provides, as a recording medium, a phosphor that absorbs and accumulates radiation and that emits stimulated emission depending on the intensity of the accumulated radiation when irradiated with excitation light after that. An image storage plate having a layer is formed into a cylindrical shape so that the phosphor layer is located on the inner peripheral surface, and a cylindrical image storage means is used. The fluorescent material on the inner peripheral surface of the image storage means is used. Accumulating an X-ray diffraction image in a layer and changing the relative positional relationship between the reading means and the erasing means for reading the image formed in the image accumulating means so that the image accumulating means can be moved. It was made possible. As a result, while an image is being stored in one place, an image that has been stored in another place before that is read, and the residual image that has already been read in another place is deleted to prepare for the next storage. It enables efficient measurement and, as a result, removes the complexity of the conventional photographic method while keeping the advantage of the conventional photographic method that a large amount of crystal information can be recorded with one exposure. Specifically, it has a phosphor layer that absorbs and accumulates radiation and that stimulates emission of light in response to the intensity of the accumulated radiation when irradiated with excitation light after that. An image storage plate is formed in a cylindrical shape so that the phosphor layer is located on the inner peripheral surface, and an X-ray passage hole penetrating the outer peripheral surface and the inner peripheral surface of the storage plate at a substantially central portion of the cylindrical shape. And an image storage means provided with The sample to be measured placed on the cylindrical surface containing the fluorescent material layer in the X-ray passing hole of the stacking portion is irradiated with X-rays, and the fluorescent material layer of the image storage means is irradiated with the X-rays of the sample. X-ray irradiation means for forming a diffraction image, image reading means for scanning the inner peripheral surface of the image storage means to read the X-ray diffraction image accumulated in the phosphor layer, and the image reading means, Erasing means arranged at intervals and erasing the image accumulated in the phosphor layer by irradiating the inner peripheral surface of the image accumulating means with light, and the image accumulating means parallel to the central axis of the cylinder. And a moving unit that moves in any direction to change the relative positional relationship between the image storage unit and the image reading unit and the erasing unit.

[Operation] In the above-mentioned configuration, the sample is irradiated with X-rays by the X-ray irradiating means, and the image accumulating means is irradiated with X-rays of the sample.
Accumulate line diffraction images. At this time, at the same time, the reading means reads the image already accumulated at another location of the image accumulating means, which is opposite to the reading position of the reading means. Further, at the same time, the residual image after completion of reading, which remains at a position other than the image storage unit and facing the erase position of the erase unit, is erased by the erase unit.

After this series of operations is completed, the moving means moves the image accumulating means to adjust the image accumulated by the operation to a position where the reading means can read the image, and the residual image in the operation. The place where is erased is aligned with the position where the X-ray diffraction image of the sample is formed.

Then, accumulation and reading are performed in the same manner as described above. At this time, if there is a residual image at a position of the image accumulating means facing the erasing position of the erasing means, the residual image is simultaneously erased by the erasing means.

Thus, according to the above configuration, accumulation of X-ray diffraction images,
Reading and erasing operations can be performed in parallel, and extremely efficient measurements can be performed.

[Embodiment] FIG. 1 is a partially broken vertical sectional view showing a main part of an X-ray diffraction apparatus according to an embodiment of the present invention, and FIG. 2 is a II in FIG.
It is a figure showing the whole X-ray diffraction device composition concerning one example of the present invention including a II cross section.

In these figures, reference numeral 1 is a cylindrical image storage plate having a fluorescent material layer formed on its inner peripheral surface.

The phosphor layer of the image storage plate 1 has a property of absorbing and accumulating radiation and stimulatingly stimulating emission of the accumulated radiation when irradiated with excitation light after that. The phosphor layer itself having such properties is known (see, for example, JP-A-59-13235).

A guide member 2 is attached to the right side of the image accumulating plate 1 in the drawing, and a guide column 4 installed upright on a base 3 is fitted to the guide member 2. Further, the guide member 2 is attached to the guide member 2. A screw rod 6 which is rotationally driven by a motor 5 fixed to the base 3 is screwed. Therefore, the image storage plate 1 is moved up and down in the drawing by rotating the screw rod 6 by the motor 5. In this case,
The guide member 2, the guide column 4, the motor 5 and the screw rod 6 constitute a moving means for moving the image storage means 1.

Further, a slit-shaped X-ray passage hole 7 is formed on the left side of the image storage plate 1 in the figure so as to penetrate the inner peripheral surface and the outer peripheral surface of the image storage plate 1. On the base 3, a cylindrical main body 8 having an inner diameter slightly larger than the outer diameter of the image accumulating plate 1 covers the image accumulating plate 1 and is arranged coaxially with the image accumulating plate 1. It is installed as.

A roof portion 9 is formed at the upper end of the main body portion 8, a mounting hole 10 is formed at the center of the roof portion 9, and the mounting hole 10 has a cylindrical shape through a bearing 11. A reading unit 12 is rotatably mounted, and a detection unit 14 fixed to the roof 9 via a mounting member 13 is mechanically separated and optically attached to the upper end of the reading unit 12. Are arranged to be coupled to. In this case, the gear 15 is fixed to the upper portion of the reading unit 12 in the main body unit 8.
A gear 16 is meshed with the gear 16, and the gear 16 is fixed to a rotary shaft of a motor 17 fixed to the inner surface of the roof 9. Therefore, by rotating the motor 17, the reading unit 12 is rotated.

The reading unit 12 is bent so that its lower end faces the inner peripheral surface of the image storage plate 1 to form a reading head unit 18, and the reading head unit 18 has an aspherical surface at its tip. lens
19 are provided. A total reflection mirror 20 is provided inside the bent portion of the reading unit 12.

Further, the detection unit 14 is coupled to the laser oscillator 22 via the optical fiber 21 in order to introduce the laser light that is the excitation light from the upper end portion to the upper end portion thereof, and the light such as the photomultiplier on the side portion thereof. The detector 23 is coupled. The optical paths of these laser beams and the incident optical path to the detector are coupled by a dichroic mirror 24 arranged so as to form an angle of 45 ° with respect to these optical paths.
The dichroic mirror has a property of transmitting the laser light and reflecting the stimulated emission light generated from the image storage plate 1. So this gives
The laser light as the excitation light can be applied to the inner peripheral surface of the image storage plate 1 through the aspherical lens 19, and the stimulated emission light generated by this irradiation can be applied to the detector.
23, and further, the reading unit 12
By rotating, the image accumulated on the entire inner peripheral surface of the image accumulating plate 1 can be read. Light-shielding plates 25 and 26 are provided at the lower end of the reading unit.

Further, an erasing lamp 27 and a erasing lamp 27 are fixed to a rotary shaft 29 via a support arm 28 at a position at a certain distance from the lower end of the reading unit 12 in the figure to drive the rotary shaft. By doing so, a motor 30 for driving the erasing lamp 27 to rotate along the inner peripheral surface of the image storage plate 1 is arranged. The motor 30 is fixed to the base 3.

Further, an X-ray introducing hole 31 is provided at a position facing the X-ray passing light 7 of the image accumulating plate 1 on the right side surface portion of the main body portion 8 in the figure, and below the X-ray introducing hole 31. A sample mounting portion 32 is provided which is formed by bending a part of the body portion 8 inward.

Then, as shown in FIG. 2, in the vicinity of the main body portion 8, the sample 33 mounted on the sample mounting portion 32 is irradiated with focused X-rays to cause the inner peripheral surface of the image storage plate 1 to be irradiated. A rotating anticathode type X-ray source for focusing diffracted X-rays and obtaining an X-ray diffraction image
34 and a curved monochromator 35 are provided. That is, the X-rays from the X-ray source 34 are the curved monochromator.
It is made monochromatic by 35, passes through the X-ray introducing hole 31, and is focused on one point on the inner peripheral surface of the image storage plate 1. Therefore, the sample 33 is placed on the sample mounting table 32.
Then, the diffracted X-rays from the sample are focused on each point on the inner peripheral surface of the image storage plate 1 to form an X-ray diffraction image. As a result, an X-ray diffraction image by the so-called focusing method can be stored in the image storage plate 1.

According to the above configuration, the X-ray diffraction image can be accumulated, read and erased as follows.

That is, first, the image storage plate 1 is lowered to the lower limit in the figure, and the erasing lamp 27 is rotationally driven to erase the residual image remaining on the upper portion of the image storage plate 1. Next, the image accumulating plate 1 is moved slightly upward so that the upper part of the image accumulating plate 1 is positioned so as to be located at a portion where the diffracted X-rays from the sample 33 are imaged. Then, the sample 33 is irradiated with X-rays by the X-ray source 34 and the curved monochromator 35, and the X-ray diffraction image of the sample 33 is accumulated in the image storage plate 1. At this time, at the same time, the erasing lamp 27 erases the residual image remaining at the position where the X-ray diffraction image is formed on the image storage plate 1.

Next, the motor 5 is driven to move the image accumulating plate 1 further upward so that the portion where the image is accumulated by the work is adjusted to a position where the reading unit 12 can read the image. The place where the residual image is erased is aligned with the position where the X-ray diffraction image of the sample is formed.

Next, the reading unit 12 is rotated while reading is performed, and at the same time, the X-ray diffraction image is accumulated in the same manner as described above.

Finally, the image storage plate 1 is moved further upward to read the X-ray diffraction image accumulated by the work.

When this series of operations is completed, the image storage plate 1 is again returned.
Is returned to the lower limit and the same work as above is repeated.

In this way, the work of accumulating, reading, and erasing the X-ray diffraction image can be performed, and a part of these works can be performed in parallel, and remarkably efficient measurement can be performed.

Therefore, according to the above-described embodiment, the advantage of the conventional photographic method that a large amount of crystal information can be recorded in one exposure can be used as it is, and the complexity of the conventional photographic method can be eliminated. Has great advantages.

In the above embodiment, the length of the image storage plate 1 as the image storage means in the cylinder axis direction is set to about three times the length required to store the X-ray diffraction image. Can be made longer, and by making the length longer, it is possible to increase the chances of performing the above-mentioned accumulation, reading, and erasing operations in parallel, and to enable more efficient operations.

[Effects of the Invention] As described in detail above, the present invention, as a recording medium, absorbs and accumulates radiation, and when irradiated with excitation light after that, stimulates emission according to the intensity of the accumulated radiation. An image accumulating plate having a phosphor layer is formed into a cylindrical shape so that the phosphor layer is located on the inner peripheral surface, and a cylindrical image accumulating means is used. X on the fluorescent layer
It is possible to change the relative positional relationship between the image accumulating means and the reading and erasing means for accumulating the line diffraction image and allowing the image accumulating means to move so as to read the image accumulated in the image accumulating means. It is the one. As a result, while the image is accumulated in one place, the image accumulated in the other place before is read,
This makes it possible to perform extremely efficient measurement by deleting the already read residual image in another place and preparing for the next accumulation. As a result, a large amount of crystal information can be recorded with one exposure. The advantages of the photographic method are used as they are, and the complexity of the conventional photographic method is eliminated.

[Brief description of drawings]

FIG. 1 is a partially cutaway vertical sectional view showing a main part of an X-ray diffractometer according to an embodiment of the present invention, and FIG. 2 is II- in FIG.
It is a figure showing the whole X-ray diffraction device composition concerning one example of the present invention including a II line section. 1 ... Image storage plate constituting image storage means, 2,4,5,6 ... Guide member constituting guide means, guide column, motor and screw rod, 7 ... X-ray passage hole, 12,14 ... ... reading section and detection section that constitute the reading means, 27 ... erasing lamp that constitutes the erasing means, 33 ... sample, 34,35 ... X-ray source and curved monochromator that constitute the X-ray irradiating means.

Claims (1)

[Claims] 1. An image storage plate comprising a phosphor layer which absorbs and stores radiation and stimulates and emits light according to the intensity of the stored radiation when irradiated with excitation light. Formed in a cylindrical shape so that the optical layer is located on the inner peripheral surface,
Image accumulating means provided with an X-ray passing hole penetrating the outer peripheral surface and the inner peripheral surface of the accumulating plate at substantially the center of the cylindrical shape, and the fluorescent light in the X-ray passing hole of the image accumulating portion. X-ray irradiation means for irradiating the sample to be measured placed on the cylindrical surface including the body layer with X-rays to form an X-ray diffraction image of the sample on the fluorescent body layer of the image storage means; An image reading unit that scans the inner peripheral surface of the storage unit to read the X-ray diffraction image stored in the phosphor layer; and an image reading unit that is arranged at a constant interval from the image reading unit. Erasing means for irradiating the peripheral surface with light to erase the image accumulated in the phosphor layer; and moving the image accumulating means in a direction parallel to the central axis of the cylinder to cause the image accumulating means and the image to move. A moving means for changing the relative positional relationship between the reading means and the erasing means. X-ray diffractometer.