JP2021179430A - Capillary holder and x-ray diffraction method using the same - Google Patents

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

The present invention relates to a capillary holder and an X-ray diffraction method using the capillary holder.

The X-ray diffractometer is an analyzer for irradiating a sample with X-rays emitted from an X-ray source, detecting diffracted X-rays reflected or transmitted from the sample, and analyzing the crystal structure of the sample. It is widely used for non-destructive analysis of various substances.

When measuring a powder sample with an X-ray diffractometer, some diffraction peaks are strongly detected because the powder particles are aligned in a predetermined crystal orientation, resulting in an error in the original crystal structure analysis and quantitative analysis of the sample. May occur.

Therefore, when measuring a powder sample, it has been proposed to fill a glass capillary with the powder sample in order to suppress the influence of particle orientation (see, for example, Patent Documents 1 and 2). Specifically, a small amount of powder sample is introduced into a glass capillary having one end sealed and filled, and then the capillary is cut to an appropriate length. Next, the capillary cut to a predetermined length is supported and fixed to the capillary holder. Then, the capillary holder is mounted on a mounting jig (for example, a goniometer head or the like), and this mounting jig is placed on the sample mounting portion of the goniometer of the X-ray diffractometer to perform measurement.

Japanese Unexamined Patent Publication No. 2005-291817 Japanese Patent No. 6001067

By the way, in the X-ray diffraction measurement using a capillary, the measurement is generally performed by a transmission method. In the transmission method, X-ray irradiation is performed while rotating the capillary around the center line in the longitudinal direction thereof, and the diffracted X-rays transmitted through the powder sample are detected while scanning the detector.

When rotating the capillary in the permeation method, if the rotation axis of the capillary deviates from the rotation axis of the goniometer and is eccentric, the detection angle position of the diffracted X-rays deviates, making it difficult to identify the crystal phase in the powder sample. Measurement accuracy may decrease due to variations in the lattice constant. Therefore, in the transmission method, it is important to rotate the capillary without eccentricity, and it is necessary to adjust the mounting angle of the capillary to the sample mounting portion so that the capillary does not tilt from the rotation axis.

Specifically, since the mounting jig for the X-ray diffractometer is configured so that the angle of the attached capillary can be adjusted, the rotation axis of the capillary rotates the goniometer after the capillary holder is attached to the mounting jig. Adjust the mounting angle of the capillary so that it matches the axis.

After adjusting the mounting angle of the capillary, the mounting jig equipped with the capillary holder is placed on the sample mounting portion of the goniometer of the X-ray diffractometer, and the mounting jig is fixed to the X-ray diffractometer by screwing. After mounting, check whether the capillary is eccentric, for example, with a CCD camera. If there is no eccentricity, the measurement is performed, but if eccentricity is confirmed, the mounting jig is removed, the mounting angle of the capillary is adjusted again, and the angle adjustment is repeated until the eccentricity disappears.

Generally, the capillary holder is configured to be fixed to the mount jig by screwing. However, in the case of screwing, the capillary holder may not be stably fixed because the screws do not engage. In particular, when the capillary holder is used frequently, the screws are worn, which makes it more difficult to fix the capillary holder. If the fixing of the capillary holder is unstable, the fixing of the capillary holder may be loosened during the measurement by the X-ray diffractometer, the rotation axis of the capillary may be eccentric, and accurate measurement may not be possible. In such a case, it is necessary to reattach the capillary and adjust the angle, which may deteriorate the measurement efficiency.

One object of the present invention is to provide a technique for improving the measurement efficiency of X-ray diffraction measurement.

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 diffractometer.
With the main body
An insertion hole provided at one end of the main body to insert and fix the capillary,
A magnet provided at the other end of the main body is provided.
A capillary holder having a structure that can be attached to the mount jig with the magnet.

A second aspect of the present invention is, in the first aspect, the first aspect.
The main body is made of a magnetic material.

A third aspect of the present invention is, in the first or second aspect,
At the other end of the main body, a recess into which the magnet can be fitted is provided.

A fourth aspect of the present invention is
The process of filling the capillary with a sample and
A step of preparing a capillary holder having a main body, an insertion hole provided at one end of the main body and for inserting and fixing the capillary, and a magnet provided at the other end of the main body.
A step of inserting and fixing a capillary filled with a sample into the insertion hole of the capillary holder, and
It comprises a step of fixing the capillary holder to which the capillary is attached to a mounting jig for an X-ray diffractometer by the magnet.
This is an X-ray diffraction method.

According to the present invention, the measurement efficiency of X-ray diffraction measurement can be improved.

1A and 1B are schematic views of a capillary holder according to an embodiment of the present invention, where FIG. 1A is a sectional view, FIG. 1B is a top view, and FIG. 1C is a bottom view. FIG. 2 is a diagram for explaining a case where the capillary is attached to the capillary holder. FIG. 3 is a diagram for explaining a case where the capillary holder according to the embodiment of the present invention is attached to the X-ray diffractometer via a mount jig. FIG. 4 is a schematic view of a capillary holder according to another embodiment of the present invention.

<One Embodiment of the present invention>
Hereinafter, a capillary holder according to an embodiment of the present invention and an X-ray diffraction method using the same will be described with reference to FIGS. 1 to 3. 1A and 1B are schematic views of a capillary holder according to an embodiment of the present invention, where FIG. 1A is a sectional view, FIG. 1B is a top view, and FIG. 1C is a bottom view. 1 (a) is a cross-sectional view when the mount jig is cut in the axial direction, FIG. 1 (b) is a top view when viewed from above of (a), and FIG. 1 (c) is a top view. It is a bottom view when viewed from the lower side of (a). FIG. 2 is a diagram for explaining a case where the capillary is attached to the capillary holder. FIG. 3 is a view for explaining a case where the capillary holder according to the embodiment of the present invention is attached to the X-ray diffractometer via a mount jig, and is a sectional view thereof.

(Capillary)
First, prior to the description of the capillary holder and the X-ray diffraction method, the capillary filled with the powder sample will be described.

The capillary is a sample container used for measuring a minute amount of powder sample with an X-ray diffractometer, and is formed of a material such as quartz glass, Lindemann glass, borosilicate glass, and soda glass. Specifically, the capillary is connected to a tubular portion with one end closed for filling the powder sample and an opening at the other end of the tubular portion, and expands outward to introduce the powder sample into the tubular portion. The funnel-shaped portion is provided with a funnel-shaped portion to be provided, and after the powder sample is introduced from the funnel-shaped portion to the tubular portion and filled, the funnel-shaped portion is cut and attached to the capillary holder.

(Capillary holder)
The capillary holder is a holder that holds the capillary. The capillary holder is arranged in the X-ray diffractometer via a mounting jig (so-called goniometer head), and the sample is introduced into the measuring unit. As shown in FIGS. 1 (a) to 1 (c), the capillary holder 10 of the present embodiment includes a main body portion 11, an insertion hole 12, and a magnet 13.

The main body 11 is formed of, for example, a metal material and is configured to be attached to a mounting jig. The material for forming the main body 11 is not particularly limited, and a material having a desired strength such as metal or plastic can be used. Among these, metal is preferable because it has a high specific gravity and high processing accuracy.

The main body 11 is provided with an insertion hole 12 on one surface thereof. The insertion hole 12 is configured so that the capillary 20 can be inserted. For example, as shown in FIG. 2, the capillary 20 is inserted into the insertion hole 12 so that the filling portion 21 of the powder sample protrudes to hold the capillary 20. be able to.

The dimensions (diameter and length) of the main body 11 may be appropriately changed according to the distance from the sample mounting portion of the X-ray diffractometer to the incident X-ray and the size of the mounting jig.

The main body 11 is provided with a magnet 13 on a surface opposite to the surface on which the insertion hole 12 is provided. In the present embodiment, the main body portion 11 is provided with a recessed portion, and the magnet 13 is provided so as to be fitted in the recessed portion. As a result, the magnet 13 is flush with the main body 11. The magnet 13 may be attached to the main body 11 as it is when the main body 11 is made of a magnetic material, but when the main body 11 is made of a non-magnetic material, for example, tape or adhesive is used. It is advisable to attach it by adhering it with an agent. Note that FIGS. 1 (a) to 1 (c) show a case where the insertion hole 12 and the recessed portion provided with the magnet 13 are connected, but the insertion hole 12 is a bottomed hole without being connected. You may.

The magnetic force of the magnet 13 is not particularly limited, and the capillary holder 10 can be stably fixed to the mount jig 30. Moreover, even if the mount jig 30 is rotated during measurement, the capillary holder 10 can be stably fixed. It may be a size that does not cause a misalignment of 10. Further, the shape of the magnet 13 is not particularly limited, and can be appropriately changed according to the shape and size of the capillary holder 10.

Since the capillary holder 10 of the present embodiment has a magnet 13, it can be magnetically attached to the mount jig 30. As described above, the capillary holder 10 has been attached to the mount jig 30 by screwing, but the screw threads are worn by repeated screwing, and the capillary holder 10 is attached to the mount jig 30. Sometimes it couldn't be fixed securely. In this respect, according to the capillary holder 10 of the present embodiment, the capillary holder 10 can be attached to the mount jig 30 by the magnetic force of the magnet 13, so that the capillary holder 10 can be securely fixed while suppressing the misalignment. Can be done. As a result, it can be introduced into the X-ray diffractometer so that the rotation axis of the capillary 20 is not eccentric.

(X-ray diffraction method)
Subsequently, the X-ray diffraction method using the above-mentioned capillary holder 10 will be described with reference to FIGS. 2 and 3.

First, a tubular capillary 20 is prepared by filling the capillary 20 with a powder sample and cutting the funnel-shaped portion thereof. Specifically, the powder sample is added little by little from the funnel-shaped portion of the capillary 20, and the powder sample is introduced into the tubular portion by tapping the capillary 20. This operation is repeated until the powder sample is in a predetermined position on the tubular portion. Then, after the powder sample is filled to a predetermined position, the space between the funnel-shaped portion and the tubular portion is cut. As a result, the capillary 20 filled with the powder sample is prepared.

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 filling portion 21 of the powder sample protrudes from the insertion hole 12. From the viewpoint of stably fixing the capillary 20, it is preferable to fix the capillary 20 and the peripheral edge portion of the insertion hole 12 with the fixing material 22. As the fixing material 22, for example, wax, an adhesive, clay, or a heat-shrinkable tube can be used. As the wax and clay, since they are easy to handle, it is preferable to use those that can be softened and deformed when touched by hand. The material of the heat-shrinkable tube is not particularly limited, and may be appropriately selected depending on the heat resistance of the capillary 20. When a heat-shrinkable tube is used, the heat-shrinkable tube may be formed into a thin tubular shape and provided between the capillary 20 and the peripheral edge of the insertion hole 12, and then heated.

Next, the capillary holder 10 holding the capillary 20 is attached to the mount jig 30. In the present embodiment, as shown in FIG. 3, the capillary holder 10 is fitted into the mounting portion 31 formed as a recess in the mount jig 30, and the capillary 20 is mounted so as to protrude. At this time, the capillary holder 10 is fixed to the mount jig 30 by a magnet 13 provided on the bottom surface thereof.

When the mount jig 30 is formed of a non-magnetic material, for example, a flat plate formed of the magnetic material is attached to the bottom of the mounting portion of the mount jig, and the capillary holder 10 is mounted via the flat plate. It is good to fix it to the tool 30. Further, from the viewpoint of fixing the capillary holder 10 more firmly, another magnet may be attached to the mounting portion 31 of the mount jig 30 and attracted by the two magnets to be fixed.

Next, the angle of the capillary 20 is adjusted so that the rotation axis of the capillary 20 is not eccentric. Specifically, the angle adjusting portion (not shown) provided on the mount 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.

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 diffractometer.

Next, using, for example, a CCD camera, it is confirmed that the rotation axis of the capillary 20 is not eccentric. After confirmation is obtained, the surface of the capillary 20 is irradiated with X-rays while rotating, and the transmitted diffracted X-rays are detected to acquire information on the powder sample filled in the capillary 20.

As described above, according to the capillary holder 10 of the present embodiment, since it can be attached to the mount jig 30 by the magnet 13, it is possible to avoid loosening of the fixing of the capillary holder 10 as in the case of screwing. .. Therefore, even when the capillary holder 10 is used repeatedly, it can be stably fixed to the mount jig 30. As a result, it is possible to prevent the rotation axis of the capillary 20 from being eccentric during measurement by the X-ray diffractometer. That is, it is possible to suppress remeasurement due to eccentricity and improve the measurement efficiency of the sample.

Although the embodiments of the present invention have been described above, the present invention is not limited to the above-described embodiments and can be variously modified without departing from the gist of the present invention.

In the above-described embodiment, when one magnet 13 is recessed in the central portion of the bottom surface of the main body portion 11 (the surface opposite to the surface on which the capillary 20 is inserted) and arranged so as to be flush with the main body portion 11. However, the number and shape of the magnets 13 are not particularly limited as long as the capillary holder 10 can be fixed to the mount jig 30 by magnetic force.

For example, two or more magnets 13 may be attached, or may be provided at the central portion or the outer edge portion of the bottom surface of the main body portion 11. Further, for example, the shape of the magnet 13 may be a ring shape, or may be arranged so as to be fitted into the outer edge portion of the bottom surface of the main body portion 11.

Further, for example, the magnet 13 may be mounted on the bottom surface of the main body 11 as shown in FIG. 4 instead of being fitted to the bottom surface of the main body 11 of the capillary holder 10 so as to be flush with each other. FIG. 4 is a schematic view of a capillary holder according to another embodiment of the present invention, and is a side view when viewed from the side surface. By providing the magnet 13 as shown in FIG. 4, the area of the magnet 13 can be increased as compared with the above-described embodiment, and the fixation of the capillary holder 10 by the magnetic force can be further strengthened.

10 Capillary holder 11 Main body 12 Insertion hole 13 Magnet 20 Capillary 21 Powder sample 22 Fixing material 30 Mounting jig 31 Mounting part 40 Goniometer 41 Sample mounting part

Claims (4)

A capillary holder that holds a capillary filled with a sample and is attached to a mounting jig for an X-ray diffractometer.
With the main body
An insertion hole provided at one end of the main body to insert and fix the capillary,
A magnet provided at the other end of the main body is provided.
A capillary holder having a structure that can be attached to the mounting jig with the magnet. The main body is made of a magnetic material.
The capillary holder according to claim 1. At the other end of the main body, a recess into which the magnet can be fitted is provided.
The capillary holder according to claim 1 or 2. The process of filling the capillary with a sample and
A step of preparing a capillary holder having a main body, an insertion hole provided at one end of the main body and for inserting and fixing the capillary, and a magnet provided at the other end of the main body.
A step of inserting and fixing a capillary filled with a sample into the insertion hole of the capillary holder, and
It comprises a step of fixing the capillary holder to which the capillary is attached to a mounting jig for an X-ray diffractometer by the magnet.
X-ray diffraction method.

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