JPH0797090B2 - X-ray diffractometer - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial application] The present invention is intended to obtain X-ray diffraction information of a sample by accumulating an X-ray diffraction image of the sample on a radiation image storage plate and reading the image. X-ray diffractometer.

[Prior Art] Conventionally, an X-ray diffraction image of a crystalline sample is accumulated in a radiation image accumulating plate and is read to obtain an X-ray diffraction image of the sample.
An X-ray diffractometer that obtains line diffraction information is known. That is, in this type of conventional X-ray diffractometer, a sample is placed on a goniometer and an X-ray emitted from an X-ray source is placed on the sample.
The radiation is irradiated from a predetermined direction, and the diffracted X-rays reflected from the sample at this time are accumulated in the radiation image accumulating plate. Then, the radiation image accumulating plate after the accumulation is stored at the image reading position of the radiation image reading device. Set to and the accumulated X
It was for reading a line diffraction image.

Such an X-ray diffractometer can take advantage of the conventional photographic method that can record accurate two-dimensional information relatively easily and quickly, and at the same time requires complicated development / fixing and reading. In recent years, it has attracted attention because it can overcome the drawback of the conventional photographic method that it is difficult to automate.

[Problems to be Solved by the Invention] However, in the measurement by the above-described conventional X-ray diffraction apparatus, even if the accumulation of one X-ray diffraction image is completed, the reading of the accumulated X-ray diffraction image is completed. During that time, there was a drawback that the next measurement could not be performed. That is, in order to use the radiation image storage plate for which one image has been stored for the next measurement, an operation of reading the stored image and erasing it is necessary, and until this operation is finished, It could not be used for the next measurement.

Therefore, the efficiency of the measurement is not always sufficient, and particularly in the case of performing time-resolved analysis of the crystal to obtain crystal information at each time point, for example, for a sample in which the crystal morphology changes momentarily. Has a certain limit in improving its time resolution.

The present invention has been made in the background described above.
It is possible to move from one X-ray diffraction image accumulation operation to the next accumulation operation without waiting time, thereby enabling extremely efficient measurement, and thus, for example, to improve time resolution in time-resolved analysis measurement of crystals. The object of the present invention is to provide an X-ray diffractometer which enables significant improvements.

[Means for Solving the Problems] The present invention has solved the above-mentioned problems by adopting the following configurations.

An X-ray goniometer that holds a sample and changes the irradiation direction of X-rays to the sample; a radiation image storage plate that stores an X-ray diffraction image generated from the sample when the sample is irradiated with X-rays; An X-ray diffractometer equipped with a radiation image reading device for reading a radiation image accumulated on an image accumulation plate, wherein first and second radiation image accumulation plates are used as the radiation image accumulation plate, and the first radiation image accumulation device is used. First, the plate is moved from the X-ray diffraction image storage position to the radiation image reading position and vice versa.
Moving mechanism and the second radiation image storage plate through a path different from the movement path of the first moving mechanism from the X-ray diffraction image storage position to the radiation image reading position, and vice versa. And a second moving mechanism for moving the radiation image reading position to the X-ray diffraction image storage position.

[Operation] In the above-described configuration, first, the first radiation image storage plate is placed at the X-ray diffraction image storage position, and the second radiation image storage plate is placed at the radiation image reading position. In this state, X-ray diffraction images are accumulated in the first radiation image reading device.

Next, when the accumulation of the X-ray diffraction image is completed, the first and second radiation image accumulation plates are moved to move the first radiation image accumulation plate on which the X-ray diffraction image is accumulated to the radiation image. At the reading position, the second radiation image storage plate is arranged at the X-ray diffraction image storage position.

Next, the next X-ray diffraction image storage operation is performed on the second radiation image storage plate, while the X-ray diffraction images previously stored on the second radiation image storage plate by the radiation image reading device are stored. Performs reading operation.

Then, when the X-ray diffraction image accumulating operation and the radiation image reading operation are completed, the first and second radiation image accumulating plates are moved to exchange the mutual arrangement relationship, and the X-ray diffraction image Accumulate and read radiographic images.

By repeating the above operation one after another, the waiting time when shifting from one X-ray diffraction image accumulation operation to the next accumulation operation can be significantly shortened. Therefore, it is possible to perform extremely efficient measurement, and thereby, for example, it is possible to significantly improve the time resolution in the time-resolved analysis measurement of crystals and the like.

[Embodiment] FIG. 1 is a perspective view showing the structure of an X-ray diffraction apparatus according to one embodiment of the present invention, FIG. 2 is a plan view of one embodiment, and FIGS. 3 and 4 show one embodiment. FIG. An embodiment will be described in detail below with reference to these drawings.

In the figure, reference numeral 1 is a sample, reference numeral 2 is an X-ray goniometer, reference numeral 31 is a first radiation image storage plate, and reference numeral 32 is a second.
The radiation image storage plate, reference numeral 4 is a radiation image reading device, and reference numeral 5 is a moving mechanism main body.

The sample 1 is a crystalline sample that causes X-ray diffraction, and is a sample in which the crystal form changes momentarily, such as a covaloxime complex that is an organic complex containing cobalt.

The X-ray goniometer 2 is a well-known X-ray goniometer capable of holding the sample 1 and setting or changing the incident direction of the irradiation X-ray x ₀ on the sample 1 to a desired direction.

The first and second radiation image storage plates 31 and 32 are obtained by applying a radiation image storage material on the surface of a substrate having a curved surface forming a part of a cylindrical body. When the radiation image storage substance is irradiated with radiation such as X-rays, the image generated by the irradiation is accumulated as a latent image, and when the latent image is irradiated with light for a predetermined excitation, it corresponds to the latent image. It has a property of emitting the emitted light. The radiation image accumulating substance itself is a known substance.

The radiation image reading device 4 is provided with a radiation image reading unit (not shown) at the tip of the rotary probe 41, while a light source of excitation light, a detection device of emitted light, and the like are provided in the reading device main body 42. It is what The rotary probe 41 is attached to the rotary shaft 42a together with the balance arm 41a. Then, the rotary probe 41 and the rotary shaft
42a guides excitation light to the tip of the rotating probe 41, and irradiates the excitation light to the radiation image storage plate.
The light emitted from 32 or 31 is emitted from the reading device body.
Light guiding means for guiding the emitted light in the device 42 is provided. Further, the means for detecting the emitted light is connected to an image processing device such as a computer.

That is, the radiation image reading device 4 draws the first or second radiation image storage plate 31 or 32 at the radiation image reading position, that is, the tip of the probe 41 when the rotating probe 41 is rotated. The radiation image storage plates 31 and 32 are arranged at positions slightly outside the circle so that the surface of the first or second radiation image storage plate 31 or 32 is located.
By scanning the surface of 31 or 32 with the rotating probe 41, the X-ray diffraction image accumulated on the radiation image accumulating plate 31 or 32 is read. During the reading, the radiation image storage plate 31 or 32 is moved continuously or intermittently so that the radiation image storage plate 31 or 32 is moved.
Appropriate control is performed so that the entire 31 or 32 is scanned.

The X-ray goniometer 2 and the radiation image reading device 4 are fixed to a base 6.

The moving mechanism body 5 includes the radiation image storage plates 31 and 32.
It is equipped with the main part of the moving mechanism.

That is, the moving mechanism main body 5 rotatably mounts the first and second screw rods 51 and 52 for driving along the longitudinal direction of the pedestal 50 on the pedestal 50 having a substantially rectangular shape, and drives them. Two rails on each side of the screw rods 51 and 52
51a, 51a and 52a, 52a are provided, and motors 51b and 5 for rotationally driving these first and second screw rods 51 and 52 are provided.
2b is provided.

The first and second moving bases 51c and 52c are mounted on the rails 51a and 52a so as to be movable on the rails 51a and 52a, respectively. Screw holes are provided in the portions, and the first and second driving screw rods 51 and 52 are screwed into these screw holes. Therefore, the first and second moving bases 51c and 52c can be moved along the longitudinal direction of the moving mechanism body 5 by controlling the rotations of the motors 51b and 52b, respectively.

The first radiographic image storage plate 3 is mounted on the first moving table 51c.
1 is fixed.

An auxiliary moving table 32a is movably attached to the second moving table 52c. That is, auxiliary rails 52d, 52d are attached on the second moving table 52c in a direction orthogonal to the longitudinal direction of the moving mechanism body 5, and the auxiliary moving table 32a is movably mounted on this rail. Has been done. The auxiliary moving base 32a is driven by a driving screw rod 52e and a motor 52f provided on the second moving base 52c. The second radiation image storage plate 32 is fixed to the auxiliary moving table 32a.

Therefore, the first radiation image storage plate 31 is movable along the longitudinal direction of the moving mechanism body 5. That is, the radiation image storage plate 31 is located at the X-ray diffraction image storage position (first radiation image storage plate in FIGS. 1 and 2) formed by the diffracted X-rays x diffracted from the sample 1. From the position where 31 is arranged) to the radiation image reading position where the accumulated image is read by the radiation image reading device 4 (the position where the second radiation image reading device 32 is arranged in FIGS. 1 and 2) It is also possible to move to the X-ray diffraction image accumulation position from the image reading position.

Further, the second radiation image storage plate 32 can be moved by the auxiliary moving base 32a in a direction orthogonal to the longitudinal direction of the moving mechanism body 5, that is, in the upper and lower directions in FIG. Also, it is movable along the longitudinal direction of the moving mechanism body 5. That is, this second
The radiation image storage plate 32 of is the first radiation image storage plate.
It is possible to move between the radiation image reading position and the X-ray diffraction image accumulation position by following a path different from the movement path of 31.

Therefore, as shown in FIGS. 3 and 4, the first radiation image storage plate at the X-ray diffraction image storage position is located.
It is smooth without any trouble to move 31 to the radiographic image reading position, and at the same time, move the second radiographic image storage plate 32 at the radiographic image reading position to the X-ray diffraction image storage position. You can do it.

The first screw rod 51, the rail 51a, the motor 51b, and the first moving base 51c constitute a first moving mechanism in the present invention, and the second screw rod 52, the rail 52a, and the motor 5 are also included.
2b and second moving base 52c, auxiliary moving base 32a, auxiliary rail 52
The d, the screw rod 52e, and the motor 52f constitute the second moving mechanism in the present invention.

According to one embodiment described above, the first radiation image storage plate
Immediately after the operation of accumulating the X-ray diffraction image on 31 is completed, the first radiation image accumulation plate 31 is immediately moved from the X-ray diffraction image accumulation position to the radiation image reading position of the radiation image reading device 4, and at the same time, The second radiation image storage plate 32, which has been arranged at the radiation image reading position, is moved to the X-ray diffraction image storage position, and the second radiation image storage plate 32 is moved.
Then, the next X-ray diffraction image can be accumulated. And
While the X-ray diffraction image is being stored in the second radiation image storage plate 32, the X-ray diffraction image previously stored in the first radiation image storage plate 31 is read and read out. It is possible to carry out the erasing work after the completion of. Therefore, by repeating this operation one after another, the waiting time when shifting from one X-ray diffraction image accumulation operation to the next accumulation operation can be significantly shortened. Therefore, it becomes possible to perform extremely efficient measurement, and for example, with respect to a covaloxime complex whose crystal morphology changes momentarily, time-resolved analysis and measurement of crystals can be performed with extremely high time resolution.

EFFECTS OF THE INVENTION As described above in detail, according to the present invention, the first radiation image storage plate is moved from the X-ray diffraction image storage position to the radiation image reading position, and vice versa. From the X-ray diffraction image storage position, the first moving mechanism for moving to the X-ray diffraction image storage position and the second radiation image storage plate are passed through a path different from the movement path of the first moving mechanism. And a second moving mechanism for moving the radiation image reading position to the X-ray diffraction image accumulating position and vice versa. By enabling the transfer from one X-ray diffraction image accumulation operation to the next accumulation operation without waiting time, extremely efficient measurement is possible and, for example, the time resolution in the time-resolved analysis measurement of crystals is significantly improved. Etc. are also possible The obtained X-ray diffractometer is obtained.

[Brief description of drawings]

FIG. 1 is a perspective view showing the configuration of an X-ray diffraction apparatus according to an embodiment of the present invention, FIG. 2 is a plan view of the embodiment, and FIGS. 3 and 4 are operation explanatory views of the embodiment. is there. 1 ... Sample, 2 ... X-ray goniometer, 4 ... Radiation image reading device, 5 ... Moving mechanism main body, 31 ... First radiation image storage plate, 32 ... Second radiation image storage plate.

Claims (1)

[Claims] 1. An X-ray goniometer that holds a sample and changes the irradiation direction of X-rays to the sample, and a radiation image storage that stores X-ray diffraction images generated from the sample when the sample is irradiated with X-rays. An X-ray diffraction apparatus including a plate and a radiation image reading device that reads a radiation image stored in the radiation image storage plate, wherein the radiation image storage plate includes first and second radiation image storage plates, and A first radiographic image storage plate is moved from the X-ray diffraction image storage position to the radiographic image reading position and vice versa.
Moving mechanism and the second radiation image storage plate through a path different from the movement path of the first moving mechanism from the X-ray diffraction image storage position to the radiation image reading position, and vice versa. And a second moving mechanism for moving the radiation image reading position to the X-ray diffraction image storage position.