JP2007171000A - X-ray crystal structure analyzer - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an X-ray crystal structure analyzer capable of highly accurate measurement even relative to various samples having different crystal sizes. <P>SOLUTION: In this X-ray crystal structure analyzer equipped with a condensing mirror 11 for focusing a generated X-ray into a point shape on a prescribed position, a sample S held on a sample holder provided on a goniometer 20 is irradiated with the X-ray generated from an X-ray generation device 10, to thereby analyze its crystal structure, and a distance variable means is provided on either or both of moving rails (guides) 15, 24 as a means for changing the relative distance between the X-ray generation device 10 and the goniometer 20, and thereby highly accurate measurement becomes possible even relative to various samples including a low-molecule large crystal. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to an X-ray diffractometer used for analyzing a three-dimensional structure of a crystal from diffraction points obtained by irradiating X-rays, and more particularly, a condensing mirror that narrows generated X-rays into a point at a predetermined position. The present invention relates to an X-ray diffraction apparatus including

  An X-ray crystal structure analyzer for analyzing the crystal structure of a single crystal sample irradiates a sample rotating with respect to a plurality of rotation axes with parallel X-rays focused on a minute cross section, and diffracts from the sample. The crystal structure is analyzed by detecting X-rays with a detector. That is, a conventional sample holding goniometer for freely rotating on four axes including the χ axis, the ω axis, and the Φ axis while holding a single crystal sample to be analyzed is disclosed in, for example, Patent Document 1 below. It is already known, and according to this, a sample holding goniometer is provided in which the goniometer and collimator do not collide even if the sample is rotated 360 ° around the ω axis.

  Further, according to Patent Document 2 below, light emitted from a scintillator having a relatively large area that generates an X-ray diffraction image on the surface by diffracted X-rays from a sample is transmitted by an optical fiber unit and detected by a CCD image sensor. An X-ray crystal structure analyzer equipped with an X-ray detection unit (two-dimensional detector) is already known.

  Furthermore, according to the following Patent Document 3, a rotary collar is provided on the basis of a goniometer mechanism, and it can be used for various other measurements in addition to an X-ray diffractometer with a relatively simple configuration. X-ray diffractometers that can also be used are already known.

JP-A-11-304999 JP 2002-116158 A Japanese Patent No. 2550382

  By the way, in the X-ray crystal structure analysis apparatus provided with the above-described sample holding goniometer, a sample to be analyzed is attached to a sample holder, for example, on a glass capillary, and the samples are independently separated on the three axes by the goniometer. And the X-ray detection unit, which is a two-dimensional detector, is set within a predetermined range with respect to the sample. In that case, in order to perform highly accurate measurement, it is necessary to irradiate the sample with X-rays having a larger beam size (so-called complete bathing).

  That is, in the structure of the X-ray crystal structure analysis apparatus including the above-described conventional technique, normally, there is only one position (point) that can be measured, and the beam size is minimized at the focusing point of the focusing mirror. In particular, in the case of a large crystal such as when analyzing a crystal structure of a low molecule, it is not possible to irradiate a sample with X-rays having a larger beam size (so-called complete bathing). It was difficult.

  In such a case, it may be possible to move the goniometer and / or the X-ray generation apparatus by providing a stage in both or both of them, however, after the movement, the operating axis of the goniometer or / and Since the operating axis of the X-ray generator needs to coincide with the X-ray, it becomes necessary to readjust. However, the goniometer or the X-ray generator described above has a problem that it is heavy and therefore takes time for readjustment. Or, in the structure known from the above-mentioned Patent Document 3, since it is necessary to mount a heavy X-ray detector on the rotatable collar, there is a problem that the gonio stage cannot be stably fixed. It was.

  Therefore, the present invention has been made in view of the above-mentioned problems in the prior art. That is, for example, even a large crystal such as a low molecular sample can be easily irradiated with X-rays having a larger beam size. An object of the present invention is to provide an X-ray crystal structure analysis apparatus that can perform measurement (so-called complete bathing), and can perform highly accurate measurement on various samples.

  Therefore, in the present invention, in order to achieve the above-described object, the X-ray source that irradiates the sample with the generated X-ray is provided with a condensing mirror that narrows the generated X-ray into a point shape at a predetermined position. A sample turntable that is held and supported rotatably about an axis provided in a plane including the X-ray incident surface of the sample, and an X-ray detector that detects diffracted X-rays from the sample. In the X-ray crystal structure analyzing apparatus, an X-ray crystal structure analyzing apparatus provided with means for changing a relative distance between the X-ray source and the sample turntable is further provided.

  In the present invention, in the X-ray crystal structure analyzing apparatus, it is preferable that the distance varying means is constituted by a moving rail, and further, the moving rail is provided by the X-ray source or the sample turntable. It is preferable to attach to one or both.

  According to the X-ray crystal structure analysis apparatus according to the present invention described above, X-rays having a beam size larger than that of a crystal of various sizes can be easily irradiated (so-called complete bath). Therefore, it is possible to provide an X-ray crystal structure analyzing apparatus capable of measuring with high accuracy even for various samples including low-molecular crystals.

  Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings.

  FIG. 1 attached herewith is a top view showing a schematic structure of an X-ray crystal structure analyzing apparatus according to an embodiment of the present invention. In this figure, reference numeral 10 denotes an X-ray source for generating X-rays irradiated on a sample. The X-ray generator which is is shown. As shown in the figure, the X-ray generator 10 is provided with a so-called condensing mirror 11 for narrowing the generated X-rays into dots at a predetermined position (point). In addition, a collimator 12 is attached to the tip portion.

  On the other hand, a sample holding goniometer 20 is arranged in the irradiation direction of the X-rays generated from the X-ray generator 10, and the sample (sample) S to be analyzed is, for example, glass in the goniometer 20. The sample is attached to the sample holder by a capillary made of the like and rotated on a plurality of rotation shafts. Thereby, the sample (sample) S is rotatably supported around an axis provided in a plane including the X-ray incident surface of the sample. Further, the goniometer 20 further includes, for example, a two-dimensional detector 30 constituted by a CCD image sensor as an X-ray detector for detecting diffracted X-rays from the sample, with the sample (sample) S as the center. It is pivotally attached.

  According to the present invention, in an X-ray source equipped with a condensing mirror, as shown in FIG. 3 attached, the diameter (size) of the X-ray beam obtained thereby is at a position before and after the condensing point. It is based on the inventor's knowledge that the diameter (size) is not point-like and changes depending on the distance.

  That is, in the present invention, a wheel, a roller, or a slide mechanism (not shown) is provided at the lower part of the X-ray generator 10, and rails (guides) 15 and 15 for movement are arranged on the floor on which the device is arranged. Has been established. On the other hand, wheels are also provided in the lower part of the goniometer 20, and rails (guides) 25 and 25 for movement are arranged on the floor on which the goniometer is arranged. The rails 15 and 25 are arranged in parallel to each other, and therefore, the relative distance between the X-ray generator 10 and the goniometer 20 can be easily changed. These rails 15 and 25 also coincide with the irradiation direction of X-rays generated from the X-ray generator 10 (that is, the mounting direction of the condenser mirror 11 and the collimator 12).

  As described above, by making the relative distance between the X-ray generator 10 and the goniometer 20 variable, as shown in FIG. The diameter (size) of the X-ray beam that converges at the condensing point by the action of 11 is made point-like for the small sample (sample) S (see FIG. 2A), while the large sample ( For the sample (S), the diameter (size) of the X-ray beam can be increased and adapted to the size (see FIG. 2B). That is, X-ray beams can be irradiated to the entire sample (so-called complete bath) from large crystals such as low-molecular-weight samples to other small crystals, enabling highly accurate measurement. . In the case of this example, the diameter of the X-ray beam is, for example, 0.2 mmφ in the case of FIG. 2A and 0.5 mmφ in the case of FIG. The moving distance “d” was 50 mm.

  In the embodiment described in detail above, the distance variable means including the moving rails 15 and 25 together with the wheel or roller or the slide mechanism (not shown) is provided to the goniometer 20 together with the X-ray generator 10. However, the present invention is not limited to this, and it is natural for those skilled in the art that the same effect can be obtained by providing only one of them.

  In the above embodiment, only the example of the distance variable means including the moving rails 15 and 25 together with the wheel (not shown) has been described. However, the present invention is not limited to this, and the relative distance between them is not limited. As long as it is variable, it can also be achieved by other means. In addition, a sensor that measures the relative distance between the X-ray generator 10 and the goniometer 20 is provided together with a drive mechanism having a motor or the like, so that it automatically moves. Would also be possible.

1 is a top view showing a schematic structure of an X-ray crystal structure analysis apparatus according to an embodiment of the present invention. It is a figure for demonstrating the state of irradiation to the sample of the X-ray beam in the said X-ray crystal structure analyzer. It is a figure which shows the relationship between the position before and behind the condensing point in the X-ray source provided with the condensing mirror, and the diameter (size) of the X-ray beam obtained there.

Explanation of symbols

DESCRIPTION OF SYMBOLS 10 X-ray generator 11 Condensing mirror 12 Collimator 15 Moving rail (guide)
20 Goniometer 25 Moving rail (guide)
30 Two-dimensional detector S Sample

Claims (4)

  An X-ray source that irradiates the sample with the generated X-rays, and a X-ray source that irradiates the sample with the generated X-rays at a predetermined position, and an X-ray incident surface of the sample. An X-ray crystal structure analyzing apparatus having a sample turntable rotatably supported about an axis provided on the X-ray source and an X-ray detector for detecting diffracted X-rays from the sample. An X-ray crystal structure analyzing apparatus comprising means for changing a relative distance between the sample rotating table and the sample rotating table.   2. The X-ray crystal structure analyzing apparatus according to claim 1, wherein the distance varying means is constituted by a moving rail.   2. The X-ray crystal structure analyzing apparatus according to claim 1, wherein the distance varying means is attached to one of the X-ray source and the sample turntable. 2. The X-ray crystal structure analyzing apparatus according to claim 1, wherein the distance varying means is attached to both the X-ray source and the sample turntable.

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