JP7596914B2 - Mounting tool and X-ray diffraction method using same - Google Patents

Description

The present invention relates to a mounting jig 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 with the capillary attached 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.

However, when the mounting jig is fixed with screws, the mounting angle of the capillary may change when the screws are tightened, for example due to vibration. In this case, it is necessary to repeat a series of steps, such as adjusting the angle of the capillary on the mounting jig and attaching it to the sample attachment part of the goniometer, until the capillary is no longer eccentric, which significantly reduces 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 mounting jig for mounting a capillary holder to a sample mounting portion of an X-ray diffraction apparatus,
A main body portion,
a mounting portion provided at one end of the main body portion for mounting the capillary holder;
a magnet provided at the other end of the main body,
A mount jig is supported and fixed to the sample mounting portion by the magnet.

A second aspect of the present invention is a method for producing a composition comprising the steps of:
When the magnet provided at the other end of the main body is a first magnet, the attachment portion is provided with a second magnet, and is configured so that the capillary holder can be fixed by the second magnet.

A third aspect of the present invention is a method for producing a composition comprising the steps of:
mounting the capillary filled with the powder sample in a capillary holder;
preparing a mounting jig including a main body, an attachment portion provided at one end of the main body for attaching the capillary holder, and a magnet provided at the other end of the main body;
a step of attaching the capillary holder to which the capillary is attached, to the attachment portion of the mounting jig;
and fixing the mount jig, to which the capillary holder is attached, to a sample mounting portion of an X-ray diffraction apparatus by the magnet.

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

FIG. 1 is a schematic diagram of a mounting jig 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 mounting jig according to an embodiment of the present invention is attached to an X-ray diffraction apparatus. FIG. 4 is a schematic cross-sectional view of a mounting jig according to another embodiment of the present invention. FIG. 5 is a diagram for explaining a mounting jig according to another embodiment of the present invention when it is attached to an X-ray diffraction apparatus. FIG. 6 is a schematic diagram of a mounting jig according to another embodiment of the present invention.

<One embodiment of the present invention>
A mounting jig according to an embodiment of the present invention and an X-ray diffraction method using the same will be described below. Prior to the description of the mounting jig and the X-ray diffraction method, a capillary for filling a powder sample and a capillary holder for holding the capillary will be described below. FIG. 1 is a schematic diagram of a mounting jig 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 the 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 a capillary holder. FIG. 3 is a view for explaining a state in which the mounting jig is attached to an X-ray diffraction device.

(Capillary)
A capillary is a sample container used to measure a minute amount of powder sample in 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.

(Capillary holder)
The capillary holder is a holder for attaching the capillary to the mounting jig. The capillary holder is, for example, as shown in FIG. 2, made of a cylindrical body having a hollow portion. One end of the capillary holder 20 has an insertion hole 21 into which the capillary 30 is inserted in the axial direction, and the capillary 30 can be held by inserting the capillary 30 into the insertion hole 21 so that the powder sample filling portion 31 protrudes. The material of the capillary holder 20 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 preferred because of its high specific gravity and high processing accuracy. The dimensions (diameter and length) of the capillary holder 20 may be appropriately changed depending on 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.

(Mounting jig)
Next, the mounting jig of this embodiment will be described with reference to the drawings.

The mounting jig is configured to be able to mount a capillary holder that holds a capillary filled with a powder sample, and the mounting jig is attached to the sample mounting portion of the X-ray diffraction device to introduce the powder sample into the X-ray diffraction device. Specifically, the mounting jig 10 of this embodiment is configured to include a main body portion 11, an attachment portion 12, and a magnet 13, as shown in FIG. 1.

The main body 11 is provided with an angle adjustment unit (not shown) that adjusts the angle of the capillary 30 attached via the capillary holder 20. The angle adjustment unit includes, for example, a rotation mechanism that rotates the capillary 30 and a translation mechanism that translates the capillary 30 in a plane perpendicular to the axial direction. The angle adjustment unit allows the rotation mechanism and the translation mechanism to rotate the capillary 30, so that the rotation axis of the capillary 30 can be aligned with the rotation axis of the goniometer so that the capillary 30 is not eccentric. The main body 11 is provided with a screw hole 14 for screwing the capillary holder 20 to be attached.

The material of the main body 11 is not particularly limited, and any material that provides 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 is provided with an attachment portion 12 at one end thereof, and is configured so that the capillary holder 20 can be attached. In this embodiment, the attachment portion 12 is configured as a recess so that the capillary holder 20 can be fitted into it. The attachment portion 12 is not limited to a recess, as long as it has a structure that can stably hold the capillary holder 20. The attachment portion 12 allows the capillary holder 20 to be attached and held so that the tip of the capillary 30 protrudes, as shown in FIG. 3.

A magnet 13 is provided on the other end of the main body 11, opposite the attachment portion 12. In this embodiment, a recess is provided in the main body 11, and the magnet 13 is fitted into the recess so that the magnet 13 is 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, it is preferable to attach the magnet 13 by gluing it with, for example, tape, adhesive, wax, etc.

The magnetic force of the magnet 13 is not particularly limited, and may be of any size that can stably fix the mounting jig 10 to the sample attachment section 41 and does not cause the mounting jig 10 to shift position 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 mounting jig 10.

The mounting jig 10 of this embodiment has a magnet 13, so it can be attached to the sample mounting section 41 of the goniometer 40 in the X-ray diffraction device by magnetic force. As described above, in conventional mounting jigs, mounting to the sample mounting section was performed by screwing, but when the screws were tightened, the mounting jig could shift and the capillary could be positioned eccentrically. In this regard, the mounting jig 10 of this embodiment can be attached by magnetic force, so that the mounting jig 10 is prevented from shifting due to screwing, and the capillary 30 can be positioned in the X-ray diffraction device so as not to be eccentric.

(X-ray diffraction measurement method)
Next, a method for performing X-ray diffraction measurement using the above-described mounting jig 10 will be described.

First, a tubular capillary 30 is prepared by filling the capillary 30 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 30, and the capillary 30 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 30 filled with a powder sample is prepared.

2, the capillary 30 is inserted into the insertion hole 21 of the capillary holder 20, and the capillary 30 is held so that the powder sample filling portion 31 protrudes from the insertion hole 21. From the viewpoint of stably fixing the capillary 30, it is preferable to fix the capillary 30 to the periphery of the insertion hole 21 with an adhesive 32. For example, wax, adhesive, clay, or heat shrink tubing can be used as the adhesive 32. 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 30. 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 30 and the periphery of the insertion hole 21, and then heat it.

Next, the capillary holder 20 holding the capillary 30 is attached to the mounting jig 10. Specifically, as shown in FIG. 3, the capillary holder 20 is fitted into the attachment portion 12 of the mounting jig 10 and attached so that the capillary 30 protrudes. After that, the capillary holder 20 is fixed to the mounting jig 10 by inserting a screw (not shown) into the screw hole 14 provided in the mounting jig 10 and pressing it against the capillary holder 20.

Next, the angle of the capillary 30 is adjusted so that the rotation axis of the capillary 30 is not eccentric. Specifically, an angle adjustment portion (not shown) in the main body portion 11 of the mounting jig 10 is used to adjust the angle of the capillary 30 so that the capillary 30 is not eccentric with respect to the rotation axis.

Next, the mount jig 10 with the capillary holder 20 attached is attached to the sample mounting portion 41 of the goniometer 40 in the X-ray diffraction device by the magnet 13. If the sample mounting portion 41 is made of a magnetic material, the mount jig 10 may be attached as is, but if the sample mounting portion 41 is made of a non-magnetic material, it is advisable to attach a flat plate (not shown) made of a magnetic material to the sample mounting portion 41 and attach the mount jig to the sample mounting portion 41 via the flat plate.

Next, for example, a CCD camera is used to confirm that the rotation axis of the capillary 30 is not eccentric. After this is confirmed, X-rays are irradiated onto the surface of the capillary 30 while rotating it, and the diffracted X-rays that pass through are detected to obtain information about the powder sample filled into the capillary 30.

As described above, according to the mounting jig 10 of this embodiment, since it can be attached to the sample attachment section 41 by the magnet 13, it is possible to avoid misalignment of the mounting jig 10 caused by screwing. Therefore, it is not necessary to repeatedly attach the mounting jig 10 until the rotation axis of the capillary 30 and the rotation axis of the goniometer 40 are aligned, which improves measurement efficiency.

<Other embodiments>
The present invention is not limited to the above-described embodiment, and various modifications can be made without departing from the spirit and scope of the present invention.

In the above embodiment, the capillary holder 20 is fixed to the mounting jig 10 by screwing, but the present invention is not limited to this, and the capillary holder 20 may be fixed by a magnet. Specifically, as shown in FIG. 4, when the magnet provided on the side of the sample mounting portion 41 of the main body portion 11 in the mounting jig 10 is the first magnet 13a, it is preferable to provide a second magnet 13b at the bottom of the mounting portion 12. With the second magnet 13b, for example, when the capillary holder 20 is made of a magnetic metal, the capillary holder 20 can be attached to the mounting jig 10 by magnetic force, and the measurement efficiency can be further improved. Also, for example, even when the capillary holder 20 is made of a non-magnetic material, a magnetic flat plate (not shown) or the like can be attached to the bottom surface of the capillary holder 20, and the capillary holder 20 can be attached to the mounting jig 10 by magnetic force via the magnetic flat plate. With this mounting jig 10, as shown in FIG. 5, the capillary holder 20 and the mounting jig 10 can be fixed by magnetic force, so screws can be omitted. It is advisable to arrange the first and second magnets 13a and 13b so that they do not repel each other.

In addition, in the above embodiment, the mounting jig 10 is directly attached to the sample mounting part 41, but it is preferable to attach another magnet to the sample mounting part 41 and attach the magnet on the sample mounting part 41 to the mounting jig 10. By attracting the two magnets, the mounting jig 10 can be fixed more firmly to the sample mounting part 41.

In the above embodiment, a single magnet 13 is placed in the center of the bottom surface of the main body 11 of the mounting jig 10 (the surface opposite the mounting portion 12 to which the capillary holder 20 is attached) so as to be flush with the main body 11. However, as long as the mounting jig 10 can be fixed to the sample attachment portion 41 by magnetic force, the number and shape of the magnets 13 are not particularly limited.

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 mounting jig 10 as shown in FIG. 6, instead of being fitted flush with the bottom surface of the main body 11. FIG. 6 is a schematic diagram of a mounting jig 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. 6, the area of the magnet 13 can be made larger than in the above-described embodiment, and the mounting jig 10 can be more firmly fixed by the magnetic force.

10 Mounting jig 11 Main body 12 Mounting portion 13 Magnet 13a First magnet 13b Second magnet 14 Screw hole 20 Capillary holder 21 Insertion hole 30 Capillary 31 Powder sample 32 Adhesive material 40 Goniometer 41 Sample mounting portion

Claims (3)

A mounting jig for mounting a capillary holder to a sample mounting portion of an X-ray diffraction apparatus,
A main body portion,
a mounting portion provided at one end of the main body portion for mounting the capillary holder;
a magnet provided at the other end of the main body,
A mount jig that is supported and fixed to the sample mounting portion by the magnet. When the magnet provided at the other end of the main body is a first magnet, the attachment portion is provided with a second magnet, and is configured so that the capillary holder can be fixed by the second magnet.
The mounting jig according to claim 1 . mounting the capillary filled with the powder sample in a capillary holder;
preparing a mounting jig including a main body, an attachment portion provided at one end of the main body for attaching the capillary holder, and a magnet provided at the other end of the main body;
a step of attaching the capillary holder to which the capillary is attached, to the attachment portion of the mounting jig;
and fixing the mount jig, to which the capillary holder is attached, to a sample mounting portion of an X-ray diffraction apparatus by the magnet.

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