JP7596915B2 - Capillary holder and X-ray diffraction method using same - Google Patents

Description

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

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 of the sample, and is widely used for non-destructive analysis of various substances.

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

In order to suppress the influence of particle orientation when measuring powder samples, it has been proposed to fill a glass capillary with the powder sample (see, for example, Patent Documents 1 and 2). Specifically, a small amount of powder sample is introduced into a glass capillary with one end sealed to fill it, and then the capillary is cut to an appropriate length. Next, the capillary cut to the specified length is supported and fixed to a capillary holder. The capillary holder is then attached to a mounting jig (e.g., a goniometer head), and this mounting jig is placed on the sample mounting section of the goniometer of the X-ray diffraction device to perform the measurement.

JP 2005-291817 A Patent No. 6001067

In X-ray diffraction measurements using a capillary, the transmission method is generally used. In this method, X-rays are irradiated while the capillary is rotated 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.

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.

Specifically, the mounting jig for the X-ray diffraction apparatus 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.

After adjusting the mounting angle of the capillary, the mounting jig with the capillary holder attached is placed on the sample mounting section of the goniometer of the X-ray diffraction instrument, and the mounting jig is fixed to the X-ray diffraction instrument with screws. After mounting, it is checked, for example with a CCD camera, whether the capillary is decentered. If there is no eccentricity, a measurement is performed, but if eccentricity is confirmed, the mounting jig is removed and the mounting angle of the capillary is adjusted again, and the angle adjustment is repeated until the eccentricity is eliminated.

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, as the capillary holder is used more frequently, the screws wear out, making it more difficult to fix the capillary holder. If the capillary holder is not fixed securely, it may come 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 measurements. In such cases, it may be necessary to reattach the capillary or adjust the angle, which may reduce measurement efficiency.

The present invention aims to provide a technology that improves the measurement efficiency of X-ray diffraction measurements.

The first aspect of the present invention is a method for producing a cellular membrane comprising the steps of:
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,
The capillary holder has a structure that allows it to be attached to the mounting jig by the magnet.

A second aspect of the present invention is a method for producing a composition comprising the steps of:
The body portion is formed from a magnetic material.

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

A fourth aspect of the present invention is a method for producing a composition comprising the steps of:
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.

The present invention can improve the measurement efficiency of X-ray diffraction measurements.

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

<One embodiment of the present invention>
A capillary holder according to an 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 an 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 an embodiment of the present invention is attached to an X-ray diffraction apparatus via a mounting jig.

(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.

A capillary is a sample container used to measure minute amounts of powder samples in an X-ray diffraction apparatus, and is made of materials such as quartz glass, Lindemann glass, borosilicate glass, and soda glass. Specifically, a capillary is configured with a tubular section with one end closed for filling with a powder sample, and a funnel-shaped section connected to the opening at the other end of the tubular section and expanding outward for introducing a powder sample into the tubular section. After the powder sample is introduced from the funnel-shaped section into the tubular section to fill it, the funnel-shaped section is cut and attached to the capillary holder.

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

The main body 11 is formed, for example, from a metal material and is configured to be attached to a mounting jig. There are no particular limitations on the material from which the main body 11 is formed, and any material that can provide the desired strength, such as metal or plastic, can be used. Among these, metal is preferred because of its high specific gravity and high processing precision.

The main body 11 has an insertion hole 12 on one side. The insertion hole 12 is configured so that a capillary 20 can be inserted. 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 the powder sample filling portion 21 protrudes.

The dimensions (diameter and length) of the main body 11 may be changed as appropriate depending on the distance from the sample attachment part to the incident X-rays in the X-ray diffraction device and the size of the mounting jig.

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, but 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.

The magnetic force of the magnet 13 is not particularly limited, and may be of any 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 may be changed as appropriate depending on the shape and size of the capillary holder 10.

The capillary holder 10 of this embodiment has a magnet 13, so it can be attached to the mounting jig 30 by magnetic force. As described above, the capillary holder 10 was previously attached to the mounting jig 30 by screwing, but repeated screwing caused the threads to wear out, and the capillary holder 10 could not be securely 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, so the capillary holder 10 can be securely 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.

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

First, a tubular capillary 20 is prepared by filling the capillary 20 with a powder sample and cutting its funnel-shaped portion. Specifically, the powder sample is added little by little through 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 has been filled up to the predetermined position, the portion between the funnel-shaped portion and the tubular portion is cut. In this way, a capillary 20 filled with a powder sample is prepared.

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 periphery of the insertion hole 12 with an adhesive 22. For example, wax, adhesive, clay, or heat shrink tubing can be used as the adhesive 22. Wax and clay are easy to handle, so it is preferable to use materials that can soften and deform when touched by hand. There is no particular restriction on the material of the heat shrink tubing, and it is preferable to select an appropriate material depending on the heat resistance of the capillary 20. When using a heat shrink tubing, it is preferable to mold the heat shrink tubing into a thin cylindrical shape and place it between the capillary 20 and the periphery of the insertion hole 12, and then heat it.

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 the mounting 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 the magnet 13 provided on its bottom surface.

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 mounting jig's attachment section, and the capillary holder 10 may be fixed to the mounting jig 30 via the flat plate. In order to more firmly fix the capillary holder 10, it is preferable to attach another magnet to the attachment section 31 of the mounting jig 30 and fix the capillary holder 10 by attracting it with the two magnets.

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 unit (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.

Next, the mounting jig 30 with the capillary holder 10 attached is attached to the sample mounting portion 41 of the goniometer 40 in the X-ray diffraction device.

Next, for example, a CCD camera is used to confirm that the rotation axis of the capillary 20 is not eccentric. After this is confirmed, X-rays are irradiated onto the surface of the capillary 20 while rotating it, and the diffracted X-rays that pass through are detected to obtain information about the powder sample filled into the capillary 20.

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, loosening of the capillary holder 10 as occurs when the capillary holder 10 is screwed can be avoided. 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, remeasurement due to eccentricity can be prevented, and the measurement efficiency of the sample can be improved.

Although the embodiments of the present invention have been described above, the present invention is not limited to the above-described embodiments, and various modifications can be made without departing from the spirit of the present invention.

In the above 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, but the number and shape of the magnets 13 are not particularly limited as long as the capillary holder 10 can be fixed to the mounting jig 30 by magnetic force.

For example, two or more magnets 13 may be attached, and may be provided in the center or outer edge of the bottom surface of the main body 11. Also, for example, the magnet 13 may be ring-shaped, and may be positioned so as to fit into the outer edge of the bottom surface of the main body 11.

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 by the magnetic force of the capillary holder 10 can be made more secure.

REFERENCE SIGNS LIST 10 capillary holder 11 main body 12 insertion hole 13 magnet 20 capillary 21 powder sample 22 adhesive material 30 mounting jig 31 attachment portion 40 goniometer 41 sample mounting portion

Claims (4)

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