Capillary holder and X-ray diffraction method using same

Abstract

To improve the measurement efficiency in X-ray diffraction measurement.SOLUTION: A capillary holder holding a capillary filled with a sample and attached to a mounting jig for an X-ray diffraction device comprises a main body, an insertion hole provided on one end of the main body into which the capillary is inserted and fixed, and a magnet provided on the other end of the main body. The capillary holder has a structure that allows mounting on the mounting jig by the magnet.SELECTED DRAWING: Figure 1

Description

[Technical field]

[0001] The present invention relates to a capillary holder and an X-ray diffraction method using the same. [Background technology]

[0002] An X-ray diffraction instrument is an analytical instrument that irradiates a sample with X-rays emitted from an X-ray source and detects diffracted X-rays reflected from or transmitted through the sample to analyze the crystal structure, etc. of the sample. It is widely used for non-destructive analysis of various materials.

[0003] When measuring powder samples with an X-ray diffractometer, the powder particles may align to a specific crystal orientation, causing some diffraction peaks to be detected strongly, resulting in errors in the analysis of the sample's original crystal structure and quantitative analysis.

[0004] Therefore, in order to suppress the influence of particle orientation when measuring a powder sample, it has been proposed to fill a glass capillary with the powder sample (see, for example, Patent Documents 1 and 2). Specifically, after a small amount of powder sample is introduced and filled into a glass capillary with one end sealed, the capillary is cut to an appropriate length. Next, the capillary cut to a predetermined length is supported and fixed to a capillary holder. Then, the capillary holder is attached to a mounting jig (e.g., a goniometer head), and this mounting jig is placed on the sample mounting portion of the goniometer of the X-ray diffraction device to perform the measurement. [Prior art documents] [Patent documents]

[0005] [Patent Document 1] JP 2005-291817 A [Patent Document 2] Patent No. 6001067 Summary of the Invention [Problem to be solved by the invention]

[0006] In X-ray diffraction measurements using a capillary, the transmission method is generally used, in which X-rays are irradiated while rotating the capillary around its longitudinal center line as the axis of rotation, and the diffracted X-rays that have passed through the powder sample are detected by scanning the detector.

[0007] When rotating the capillary in the transmission method, if the rotation axis of the capillary is misaligned with the rotation axis of the goniometer, the detection angle position of the diffracted X-rays will shift, making it difficult to identify the crystal phase in the powder sample and causing variations in the lattice constant, which may result in low measurement accuracy. Therefore, in the transmission method, it is important to rotate the capillary without eccentricity, and the attachment angle of the capillary to the sample attachment part must be adjusted so that the capillary does not tilt from the rotation axis.

[0008] Specifically, the mounting jig for the X-ray diffraction instrument is configured so that the angle of the attached capillary can be adjusted, so after attaching the capillary holder to the mounting jig, the mounting angle of the capillary is adjusted so that the rotation axis of the capillary coincides with the rotation axis of the goniometer.

[0009] After adjusting the capillary attachment angle, the mount jig with the capillary holder attached is placed on the sample attachment section of the goniometer of the X-ray diffraction instrument, and the mount jig is fixed to the X-ray diffraction instrument with screws. After attachment, it is checked, for example with a CCD camera, whether the capillary is decentered or not. If there is no decentering, measurements are performed, but if decentering is confirmed, the mount jig is removed and the capillary attachment angle is adjusted again, and the angle adjustment is repeated until there is no decentering.

[0010] Generally, the capillary holder is configured so that it can be fixed to the mounting jig by screwing. However, when screwing, the screws may not mesh and the capillary holder may not be stably fixed. In particular, when the capillary holder is used frequently, the screws wear out and it becomes more difficult to fix the capillary holder. If the fixation of the capillary holder is unstable, the fixation of the capillary holder may become loose during measurement with the X-ray diffraction device, causing the rotation axis of the capillary to become eccentric, making it impossible to perform accurate measurement. In such a case, it may be necessary to reattach the capillary or adjust the angle, which may reduce the measurement efficiency.

[0011] An object of the present invention is to provide a technique for improving the measurement efficiency of X-ray diffraction measurement. [Means for solving the problem]

[0012] The first aspect of the present invention is A capillary holder that holds a capillary filled with a sample and is attached to a mounting jig for an X-ray diffraction apparatus, A main body portion, an insertion hole provided at one end of the body portion into which the capillary is inserted and fixed; a magnet provided at the other end of the main body, The capillary holder has a structure that allows it to be attached to the mounting jig by the magnet.

[0013] The second aspect of the present invention is the method according to the first aspect, The body portion is formed from a magnetic material.

[0014] A third aspect of the present invention is the method according to the first or second aspect, The other end of the main body is provided with a recess into which the magnet can be fitted.

[0015] A fourth aspect of the present invention is filling the capillary with a sample; preparing a capillary holder including a main body, an insertion hole provided at one end of the main body into which the capillary is inserted and fixed, and a magnet provided at the other end of the main body; inserting and fixing a capillary filled with a sample into the insertion hole of the capillary holder; and fixing the capillary holder to which the capillary is attached to a mount jig for an X-ray diffraction apparatus by the magnet. This is an X-ray diffraction method. Effect of the Invention

[0016] According to the present invention, it is possible to improve the measurement efficiency of X-ray diffraction measurement. [Brief description of the drawings]

[0017] [Figure 1] FIG. 1 is a schematic diagram of a capillary holder according to one embodiment of the present invention, where (a) is a cross-sectional view, (b) is a top view, and (c) is a bottom view. [Diagram 2] FIG. 2 is a diagram for explaining the state when the capillary is attached to the capillary holder. [Diagram 3] FIG. 3 is a diagram for explaining a state in which a capillary holder according to an embodiment of the present invention is attached to an X-ray diffraction apparatus via a mounting jig. [Figure 4] FIG. 4 is a schematic diagram of a capillary holder according to another embodiment of the present invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0018] <One embodiment of the present invention> A capillary holder according to one embodiment of the present invention and an X-ray diffraction method using the same will be described below with reference to Figs. 1 to 3. Fig. 1 is a schematic diagram of a capillary holder according to one embodiment of the present invention, in which (a) is a cross-sectional view, (b) is a top view, and (c) is a bottom view. Fig. 1(a) is a cross-sectional view of a mounting jig cut in the axial direction, Fig. 1(b) is a top view as viewed from above (a), and Fig. 1(c) is a bottom view as viewed from below (a). Fig. 2 is a view for explaining a state in which a capillary is attached to the capillary holder. Fig. 3 is a cross-sectional view for explaining a state in which a capillary holder according to one embodiment of the present invention is attached to an X-ray diffraction device via a mounting jig.

[0019] (Capillary) First, before describing the capillary holder and the X-ray diffraction method, the capillary into which the powder sample is filled will be described.

[0020] A capillary is a sample container used to measure a minute amount of powder sample with an X-ray diffraction apparatus, and is made of materials such as quartz glass, Lindemann glass, borosilicate glass, soda glass, etc. Specifically, a capillary is configured to include a tubular portion with one end closed for filling with a powder sample, and a funnel-shaped portion connected to the opening at the other end of the tubular portion and expanding in diameter toward the outside for introducing the powder sample into the tubular portion, and after the powder sample is introduced from the funnel-shaped portion into the tubular portion to fill the capillary, the funnel-shaped portion is cut and attached to a capillary holder.

[0021] (Capillary holder) The capillary holder is a holder that holds a capillary. The capillary holder is placed in an X-ray diffraction device via a mounting jig (so-called goniometer head), and introduces a sample into a measurement unit. The capillary holder 10 of this embodiment is configured to include a main body 11, an insertion hole 12, and a magnet 13, as shown in Figures 1(a) to 1(c).

[0022] The main body 11 is formed, for example, from a metal material and is configured to be attached to a mounting jig. The material from which the main body 11 is formed is not particularly limited, and any material that can provide the desired strength, such as metal or plastic, can be used. Among these, metal is preferable because of its high specific gravity and high processing accuracy.

[0023] The main body 11 has an insertion hole 12 on one surface thereof. The insertion hole 12 is configured so that a capillary 20 can be inserted therein, and for example, as shown in Fig. 2, the capillary 20 can be held by inserting the capillary 20 into the insertion hole 12 so that a portion 21 filled with a powder sample protrudes.

[0024] The dimensions (diameter and length) of the main body 11 may be appropriately changed according to the distance from the sample mounting portion to the incident X-rays in the X-ray diffraction device and the size of the mounting jig.

[0025] The magnet 13 is provided on the surface of the main body 11 opposite to the surface on which the insertion hole 12 is provided. In this embodiment, a recess is provided in the main body 11, and the magnet 13 is provided so as to fit into the recess. This makes the magnet 13 flush with the main body 11. When the main body 11 is made of a magnetic material, the magnet 13 may be attached directly to the main body 11. When the main body 11 is made of a non-magnetic material, the magnet 13 may be attached by adhering it with, for example, tape or adhesive. Note that although FIGS. 1(a) to (c) show a case in which the insertion hole 12 and the recess in which the magnet 13 is provided are connected, the insertion hole 12 may be a hole with a bottom without being connected.

[0026] The magnetic force of the magnet 13 is not particularly limited, and may be of a size that can stably fix the capillary holder 10 to the mounting jig 30 and does not cause the capillary holder 10 to shift position even when the mounting jig 30 is rotated during measurement. The shape of the magnet 13 is also not particularly limited, and can be changed as appropriate depending on the shape and size of the capillary holder 10.

[0027] The capillary holder 10 of this embodiment has the magnet 13, and therefore can be attached to the mounting jig 30 by magnetic force. As described above, the capillary holder 10 has been attached to the mounting jig 30 by screwing in the past, but repeated screwing wears the threads, and the capillary holder 10 cannot be reliably fixed to the mounting jig 30. In this regard, the capillary holder 10 of this embodiment can be attached to the mounting jig 30 by the magnetic force of the magnet 13, and therefore the capillary holder 10 can be reliably fixed while suppressing its positional deviation. As a result, the capillary 20 can be introduced into the X-ray diffraction device without eccentricity of the rotation axis.

[0028] (X-ray diffraction method) Next, an X-ray diffraction method using the above-mentioned capillary holder 10 will be described with reference to FIGS.

[0029] First, the capillary 20 is filled with a powder sample and its funnel-shaped portion is cut to prepare a tubular capillary 20. Specifically, the powder sample is added little by little from the funnel-shaped portion of the capillary 20, and the capillary 20 is tapped to introduce the powder sample into the tubular portion. This operation is repeated until the powder sample reaches a predetermined position in the tubular portion. Then, after the powder sample is filled up to the predetermined position, the portion between the funnel-shaped portion and the tubular portion is cut. In this way, the capillary 20 filled with the powder sample is prepared.

[0030] Next, as shown in FIG. 2, the capillary 20 is inserted into the insertion hole 12 of the capillary holder 10, and the capillary 20 is held so that the powder sample filling portion 21 protrudes from the insertion hole 12. From the viewpoint of stably fixing the capillary 20, it is preferable to fix the capillary 20 to the peripheral portion of the insertion hole 12 with an adhesive 22. As the adhesive 22, for example, any of wax, adhesive, clay, and heat shrink tubing can be used. As for the wax and clay, since they are easy to handle, it is preferable to use materials that can be softened and deformed when touched by hand. As for the heat shrink tubing, the material is not particularly limited, and it is preferable to select an appropriate material according to the heat resistance of the capillary 20. When using a heat shrink tubing, it is preferable to heat the heat shrink tubing after forming it into a thin cylindrical shape and providing it between the capillary 20 and the peripheral portion of the insertion hole 12.

[0031] Next, the capillary holder 10 holding the capillary 20 is attached to the mounting jig 30. In this embodiment, as shown in Fig. 3, the capillary holder 10 is fitted into an attachment portion 31 formed as a recess in the mounting jig 30, and is attached so that the capillary 20 protrudes. At this time, the capillary holder 10 is fixed to the mounting jig 30 by a magnet 13 provided on the bottom surface thereof.

[0032] When the mounting jig 30 is made of a non-magnetic material, for example, a flat plate made of a magnetic material may be attached to the bottom of the attachment part of the mounting jig, and the capillary holder 10 may be fixed to the mounting jig 30 via the flat plate. From the viewpoint of fixing the capillary holder 10 more firmly, it is preferable to attach another magnet to the attachment part 31 of the mounting jig 30 and fix the capillary holder 10 by attracting the two magnets.

[0033] Next, the angle of the capillary 20 is adjusted so that the rotation axis of the capillary 20 is not eccentric. Specifically, an angle adjustment part (not shown) provided on the mounting jig 30 is used to adjust the angle of the capillary 20 so that the capillary 20 is not eccentric with respect to the rotation axis.

[0034] Next, the mounting jig 30 to which the capillary holder 10 is attached is attached to the sample mounting portion 41 of the goniometer 40 in the X-ray diffraction apparatus.

[0035] Next, for example, a CCD camera is used to confirm that the rotation axis of the capillary 20 is not eccentric. After confirmation, X-rays are irradiated onto the surface of the capillary 20 while rotating the capillary 20, and the diffracted X-rays that pass through are detected to obtain information on the powder sample filled in the capillary 20.

[0036] As described above, according to the capillary holder 10 of this embodiment, since it can be attached to the mounting jig 30 by the magnet 13, it is possible to prevent the capillary holder 10 from loosening as occurs in the case of screw fastening. Therefore, even if the capillary holder 10 is used repeatedly, it can be stably fixed to the mounting jig 30. As a result, it is possible to prevent the rotation axis of the capillary 20 from becoming eccentric during measurement with the X-ray diffraction device. In other words, it is possible to prevent remeasurement due to eccentricity and improve the measurement efficiency of the sample.

[0037] Although an embodiment of the present invention has been described above, the present invention is not limited to the above-described embodiment, and various modifications can be made without departing from the spirit of the present invention.

[0038] In the above-described embodiment, a single magnet 13 is recessed into the center of the bottom surface of the main body 11 (the surface opposite to the surface into which the capillary 20 is inserted) and positioned flush with the main body 11. However, as long as the capillary holder 10 can be fixed to the mounting jig 30 by magnetic force, the number and shape of the magnets 13 are not particularly limited.

[0039] For example, two or more magnets 13 may be attached, and may be provided at the center or outer edge of the bottom surface of main body 11. Furthermore, for example, magnet 13 may be ring-shaped, and may be disposed so as to fit into the outer edge of the bottom surface of main body 11.

[0040] Also, for example, the magnet 13 may be attached to the bottom surface of the main body 11 of the capillary holder 10 as shown in Fig. 4, instead of being fitted flush with the bottom surface of the main body 11. Fig. 4 is a schematic diagram of a capillary holder according to another embodiment of the present invention, and is a side view when viewed from the side. By providing the magnet 13 as shown in Fig. 4, the area of ​​the magnet 13 can be made larger than in the above-mentioned embodiment, and the fixation of the capillary holder 10 by the magnetic force can be made stronger. [Explanation of symbols]

[0041] 10 Capillary holder 11 Main body 12 Insertion hole 13. Magnet 20 Capillary 21 Powder sample 22 Adhesive 30 Mounting fixture 31 Mounting part 40 Goniometer 41 Sample attachment section

Claims

1. A capillary holder that holds a capillary filled with a sample and is attached to a mounting jig for an X-ray diffraction apparatus, comprising: A main body portion, an insertion hole provided at one end of the body portion into which the capillary is inserted and fixed; a magnet provided at the other end of the main body, A capillary holder having a structure that allows it to be attached to the mounting jig by the magnet.

2. The body portion is formed from a magnetic material. The capillary holder of claim 1 .

3. The other end of the main body is provided with a recess into which the magnet can be fitted.

3. A capillary holder according to claim 1 or 2.

4. filling the capillary with a sample; preparing a capillary holder including a main body, an insertion hole provided at one end of the main body into which the capillary is inserted and fixed, and a magnet provided at the other end of the main body; inserting and fixing a capillary filled with a sample into the insertion hole of the capillary holder; and fixing the capillary holder to which the capillary is attached to a mount jig for an X-ray diffraction apparatus by the magnet. X-ray diffraction methods.

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