JPH10115596A - Sample holder for x-ray diffratometer and sample fixation method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a sample holder, for an X-ray diffractometer, and a sample fixation method which simplify an operation to fix a sample to the sample holder in such a way that a sample measuring face and the surface of the sample holder are on the same plane. SOLUTION: A fixed base 1 which is provided with a sample sandwiching face 2 and a moving base 5 which is provided with a sample sandwiching face 7 are installed, an rods 4 which comprise thread grooves 3 are fixed to the sample sandwiching face 2 at the fixed base 1 so as to protrude. The moving face 5 is inserted into, and passed through, the rods 4 in such a way that the sample sandwiching face 7 is faced with the sample sandwiching face 2 at the fixed base 1, nuts 8 are screwed, and a sample holder, for an X-ray diffractometer, which fixes a sample is formed. Taper faces which are force-fitted to the moving base 5 may be formed at edges of the nuts 8 so that the dislocation of the rods 4 from through holes in the moving base 5 is prevented and that a sample measuring face and the surface of the sample holder are the same plane. In addition, when the sample is a powder, adhesive fixation body in which an adhesive material is filled into a box body is used, and the sample can be fixed easily to the sample holder.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sample holder for fixing a sample when performing analysis with an X-ray diffractometer and a method for fixing a sample using the sample holder.

[0002]

2. Description of the Related Art An X-ray diffractometer is a device for examining the types of molecules constituting a sample. The schematic configuration of the device is as shown in FIG.
, And emits an electron beam from the electron source 23 to impinge on a target 24 made of a pure substance.
X-rays are diffracted by the sample, and the X-rays are detected by the X-ray detector 25, whereby the types of molecules constituting the sample can be determined. At this time, the sample, the target 24 and the X-ray detector 25
Are on the common Rowland circle R, which is a condition for diffracting X-rays by the sample.

As shown in FIG. 13, conventionally, a sample holder 21 for fixing a sample is provided with a through hole in a part of a main body 26 made of a metal plate to form a holding hole 27, and the sample is placed in the holding hole 27. This is a configuration for holding. Here, in the sample holder 21, the surface that becomes the front side when placed on the sample stage 22 is the upper surface 2.
8 is assumed.

Here, a method for fixing a sample to the sample holder 21 will be described. When the sample is a fine powder, the sample holder 21 is placed in a direction in which the upper surface 28 abuts on a flat table, and the sample is packed in the holding hole 27 and pressed to fix the sample in the holding hole 27. At this time, since the sample is pressed and fixed to the flat table, the surface in contact with the flat table becomes a flat surface, and the sample holder 21 in contact with the flat table becomes flush with the surface. It is fixed to the sample table 22 as a sample measurement surface. When the sample is a solid, as shown in FIG. 14, the sample is placed on a flat table with the upper surface 28 of the sample holder 21 down, the sample A is placed in the holding hole 27, and an adhesive tape 29 (clay may be used). ) To fix the sample A to the sample holder 21. At this time, as shown in FIG. 15, the sample measurement surface B of the sample A is a plane, and since the sample measurement surface B and the upper surface 28 of the sample holder 21 are in contact with a flat table, they are on the same plane. Then, the sample holder 21 is turned over and fixed to the sample table 22.

Further, when the sample A is a fine powder, the sample A cannot be fixed unless the amount of the sample A is sufficient for the holding hole 27, so that a small amount of the sample A can be fixed. A sample holder 21 ′ having a holding hole 27 ′ having a bottom surface 30 shown in FIG. 16 has been proposed.

A method for fixing the fine powder sample A to the sample holder 21 'will be described. The sample holder 21 ′ is placed on a table with the upper surface 28 facing up, and the sample A is inserted into the holding hole 27 ′.
Is filled and fixed, and the sample A is scraped and flattened using a spatula or the like so that the sample A is flush with the upper surface 28.
Further, when the amount of the sample A is not enough to fill the holding hole 27 ′, as shown in FIG. 17 and FIG.
A double-sided tape 31 is attached to the bottom surface 30 of the holding hole 27 ′ so as to be substantially flush with the upper surface 28, and the sample A is adhered and fixed on the double-sided tape 31.
Glue 32 into holding hole 27 ′ so that
The sample A is adhered and fixed to the surface of the paste 32.

[0007]

When a sample is measured by an X-ray diffractometer, the sample A is diffracted by the sample A and detected by the X-ray detector 25. The sample A must be positioned on the Rowland circle R in FIG. 12 with the surface being a plane and the upper surface 28 of the sample holder 21 and the sample measurement surface being the same plane.

When the sample A is fixed to the sample holder 21 (see FIG. 13) having the above-described through hole holding hole 27,
There are the following problems that complicate the measurement operation. When the sample A is a fine powder, since the sample A is packed in the holding hole 27 and pressed and fixed as described above, the sample A can be temporarily formed into a flat surface. There is a problem that the surface is shifted. Further, there is an annoyance that the sample A, which is a fine powder, must be fixed to the holding hole 27.

On the other hand, in the case of the solid sample A, the holding hole 2
In the case of a sample larger than 7, the sample must be cut and processed. When the sample holder 21 is placed and fixed so that the upper surface 28 of the sample holder 21 is in contact with the flat table as described above, the sample measurement surface B and the upper surface 28 are turned over because the sample holder 21 is turned over for measurement. There is a problem of shifting. When the thickness of the sample A is too thin or too thick, it is difficult to fix the sample measurement surface B of the sample A and the upper surface 28 of the sample holder 21 with the adhesive tape 29 or the like so as to keep the same plane. .

Further, when the sample A is fixed to the sample holder 21 '(see FIG. 16) having the holding hole 27' having the bottom surface 30, there are the following problems. When the sample A is fixed to the sample holder 21 ′, the fine powder sample A is pressed and fixed in the holding hole 27 ′, and the sample A is cut off with a spatula or the like so that the sample A is flush with the upper surface 28. Because
Although the sample A can be made flat and the bottom surface 30 is used, the sample A is relatively hard to collapse. However, in order to actually cut the sample A with a spatula or the like so as to be flush with the upper surface 28, the sample A The diameter must be less than about 1 μm. For this reason, there is a limit on the sample A that can be fixed to the sample holder 21 ′.

As shown in FIG. 17, when the double-sided tape 31 is used, it is difficult to make the upper surface thereof flat, and when the particle size of the sample A is large, it is larger than that of the upper surface 28. Since it protruded upward, it was impossible to measure accurately. Also, as shown in FIG.
In the case where 2 is filled in the holding hole 27 ', there is a problem that this filling operation is very difficult.

Accordingly, the present invention simplifies the operation of fixing the sample A to the sample holders 21 and 21 'so that the sample measurement surface B of the sample A and the upper surface 28 of the sample holders 21 and 21' are flush with each other. An object of the present invention is to provide a sample holder for an X-ray diffractometer and a sample fixing method.

[0013]

In order to achieve the above object, according to the first aspect of the present invention, a plurality of rods each including a fixed table and a movable table each having a sample holding surface and having a thread groove are provided. The movable table is fixed to the sample holding surface of the fixed table so as to protrude at a predetermined distance, and the movable table is inserted through the rod so that the sample holding surface of the movable table faces the sample holding surface of the fixed table. A sample holder for an X-ray diffractometer, comprising a nut screwed into the sample holder.

According to a second aspect of the present invention, in the configuration of the first aspect, the end surface of the nut is formed in a tapered surface so as to press-fit the movable table.
It is a sample holder for a line diffraction apparatus.

According to the third aspect of the present invention, the rod provided on the sample holding surface of the fixed table is inserted so as to face the sample holding surface of the movable table, and is mounted on a flat table. The sample is placed between the sample holding surface of the table and the movable table, and then the nut is screwed into the rod, and the nut is tightened so that the tip of the tapered surface provided on the nut is pressed into the movable table. This is the method for fixing the sample.

According to a fourth aspect of the present invention, in the method according to the third aspect, the sample is fixed to an adhesive fixed body filled with an adhesive member in a box having a side surface height equal to the sample holding surface. It is characterized by being.

[0017]

DESCRIPTION OF THE PREFERRED EMBODIMENTS As an embodiment of the present invention based on claim 1, a sample holder for an X-ray diffraction apparatus according to the present invention is shown in FIG.
As shown in FIG. 1, a rod 4 having a thread groove 3 is fixed so as to protrude from the sample holding surface 2 of the fixed base 1, and the sample holding surface 7 of the movable base 5 is opposed to the sample holding surface 2 of the fixed base 1. The sample is fixed by inserting the movable table 5 through the rod 4 and screwing the nut 8. As described above, since the fixed base 1 and the movable base 5 are formed of different members, the sample is placed between the sample holding surfaces 2 and 7 without aligning the sample with the holding hole 27 as in the conventional sample holder 21. And screw the nut 8 into place. Therefore, the work of fixing the sample to the sample holder becomes easy.

As an embodiment of the invention based on claim 2, the end face of the nut 8 forms a tapered surface 9 that is press-fitted into the movable base 5 as shown in FIG. With such a configuration, the displacement of the through hole 6 of the movable base 5 and the rod 4 can be prevented, so that the movable base 5 is stabilized.

According to an embodiment of the present invention, the rod 4 provided on the sample holding surface 2 of the fixed table 1 is inserted into the movable table 5 so as to face the sample holding surface 7 and is placed on a flat table. And then the sample holding surfaces 2 of the fixed table 1 and the movable table 5
7, the nut 8 is screwed into the rod 4, and the nut 8 is tightened so that the tip of the tapered surface 9 provided on the nut 8 is pressed into the movable base 5.
The sample is securely fixed, and the sample and the upper surface of the sample holder are flush with each other.

As an embodiment based on claim 4, as shown in FIG. 9, a sample A has an adhesive member 17 filled in a box 18 having a side surface height equal to the sample holding surfaces 2 and 7. It is fixed to the fixed body 16. Thereby, even if the sample A is a powder, it can be fixed to the sample holder.

A sample holder for an X-ray diffraction apparatus according to the present invention will be described with reference to the accompanying drawings. 1 and 2, one side surface of a fixing table 1 is used as a sample holding surface 2, and two rods 4 having screw grooves 3 are fixed to the sample holding surface 2 so as to protrude at a predetermined distance. A through hole 6 through which the rod 4 can be inserted is provided on a side surface of the movable base 5 having the same thickness as the fixed base 1.
And one surface having the through hole 6 is used as a sample holding surface 7. The movable table 5 is positioned so that the sample holding surface 7 and the sample holding surface 2 face each other, and is inserted into the rod 4. A nut 8 is screwed into the rod 4. As shown in FIG. 2, the nut 8 has a tapered surface 9 on the side facing the movable table 5, and a peripheral edge of the tip is inserted into the through hole 6 of the movable table 5.
For this reason, the diameter of the through hole 6 is such that the entire tapered surface 9 of the nut 8 or a part of the tapered surface 9 can be inserted.

Since the movable table 5 is movably inserted into the rod 4, the movable table 5 normally swings, and the height thereof becomes unstable. However, in the sample holder of the present invention, since the tapered surface 9 is provided on the nut 8, the peripheral edge of the tapered surface 9 is press-fitted into the through hole 6 of the movable base 5 to fix the movable base 5, so that the height is stable. The fixed table 1, the movable table 5, and the sample measurement surface B can be coplanar.

A method for fixing a sample using the sample holder for an X-ray diffraction apparatus of the present invention having the above-described structure will be described below. The case where the sample A is a solid as shown in FIG. 3 will be described. First, the nut 8 is loosened, the movable table 5 is positioned on the free end side of the rod 4, and a predetermined interval is provided between the sample holding surfaces 2 and 7 of the fixed table 1 and the movable table 5, respectively. Place on a table. Subsequently, the sample A is placed on both sample holding surfaces 2,
Between 7, the sample measurement surface B is placed so as to be in contact with the flat table. Then, screw the nut 8 into the rod 4,
The periphery of the distal end of the tapered surface 9 provided on the nut 8 is
The sample A is fixed while being press-fitted into the through hole 6 of FIG. At the time of sample measurement, as shown in FIG. 3, the sample holder is turned upside down so that the sample measurement surface B is on the upper surface, and the sample table 22 (see FIG. 12).
Should be fixed to.

Further, as shown in FIG.
Irregularities may be provided on the sample holding surface 7 (similarly), and the friction surface 10 may be provided. When the friction surface 10 is provided in this manner, the sample A
The friction between the sample holding surfaces 2 and 7 causes the sample A to be fixed more reliably. At this time, the friction surface 10 may be directly processed on the sample holding surfaces 2 and 7, or a cloth such as felt or rubber may be attached to the sample holding surfaces 2 and 7.

The sample holder shown in FIG.
A notch 7 is formed to form a locking groove 11. By providing the locking grooves 11 on the sample holding surfaces 2 and 7 as described above, a part of the sample A is locked in the locking grooves 11, so that the sample A can be more securely fixed.

FIG. 6 shows a structure in which a locking wall 12 is provided on the fixed base 1 and the movable base 5 in order to increase the area of the sample holding surfaces 2 and 7. By providing the locking wall 12, the contact surface between the sample A and the sample holding surfaces 2 and 7 increases, so that the sample A having a somewhat thick thickness can be reliably held. When measuring the sample A, the sample holder is placed on a flat table in the direction shown in FIG. 6, and the sample holding surface 2 is set so that the sample measurement surface B of the sample A contacts the flat table. , 7 are mounted, and nut 8 is screwed. At the time of sample measurement, the sample holder may be turned upside down so that the sample measurement surface B is the upper surface, and fixed to the sample table 22 (see FIG. 12).

The sample holder shown in FIG.
An engaging piece 13 is provided on the sample holding surface 2 so as to protrude in parallel with the rod 4, a guide groove 14 is formed inside the engaging piece 13, and a groove is formed on a side surface of the movable base 5 corresponding to the guide groove 14. Joint 1
5 is given. In the case of such a sample holder, the groove engaging portion 15 of the movable table 5 is
, The fixed table 1 and the movable table 5 are always on the same plane. Therefore, when the sample holder having such a configuration is used, the nut 8 does not need to be provided with a tapered surface.

Next, the case where the fine powder sample A is fixed will be described. First, the adhesive fixing body 16 for fixing the fine powder sample A will be described with reference to FIG. The adhesive fixing body 16 includes an adhesive member 17 for fixing the sample A and a box 18 for holding the adhesive member 17. As shown in FIG. 9, the height of the side surface of the box 18 is formed to be the same as the height of the sample holding surfaces 2 and 7 of the fixed table 1 and the movable table 5, and an adhesive member 17 is provided inside the box 18. Will be filled.

When the sample A is fixed to the above-mentioned adhesive fixing body 16, an appropriate amount of the sample A may be placed on the adhesive member 17, and the sample A may be pressed from above with a flat spatula or the like. At this time, since the height of the side surface of the box 18 is formed equal to the sample holding surfaces 2 and 7, the sample A pressed by a spatula or the like is used.
Is on the same plane as the fixed base 1 and the movable base 5. Thus, the sample A can be placed on the adhesive member 17 and pressed down from above with a flat spatula or the like, so that even a small amount of the sample A can be fixed. Further, even when the particle size of the sample A is large, the sample A can be fixed by pressing the adhesive member 17 with a spatula or the like. Therefore, any powder sample A can be fixed to the adhesive fixing body 16.

The case where the adhesive fixed body 16 having the powder sample A fixed on the upper surface thereof is fixed to the sample holder for the X-ray diffraction apparatus of the present invention will be described below. First, the nut 8 is loosened, the movable table 5 is positioned on the free end side of the rod 4, and a predetermined interval is provided between the sample holding surfaces 2 and 7 of the fixed table 1 and the movable table 5, respectively.
The sample holder of the present invention is placed on a flat table. Subsequently, as shown in FIG. 9, the adhesive fixing body 16 is placed between the sample holding surfaces 2 and 7 with the surface on which the sample A is fixed facing upward, and the nut 8 is screwed into the rod 4. Then, the pressure-sensitive adhesive fixing body 16 is fixed while the peripheral edge of the tip end of the tapered surface 9 provided on the nut 8 is pressed into the through hole 6 of the movable base 5.

At this time, the size of the adhesive fixing body 16 is set between the sample holding surfaces 2 and 7 of the sample holder for the X-ray diffraction device of the present invention, and is sufficiently larger than the X-ray irradiation area of the X-ray diffraction device. It is preferable that the height is large, and the height of the adhesive fixing body 16 is formed equal to the sample holding surfaces 2 and 7. By making the height of the sample fixing body 16 equal to the height of the sample holding surfaces 2 and 7 in this manner, the upper surface of the sample fixing body 16 and the upper surface of the sample holder can be made the same plane. The adhesive fixed body 16 as a prototype had a bottom surface of 15 mm × 15 mm and a height of 2 mm (the thickness of the sample holding surfaces 2 and 7 of the sample holder for the X-ray diffraction apparatus of the present invention was 2 mm).

Further, when the box 18 of the adhesive fixing body 16 is made of inexpensive resin or the like and is filled with the adhesive members 17 in advance, the disposable adhesive fixing body 16 can be used. At this time, as shown in FIG. 10, if the adhesive member 17 is kept covered with paper 19 coated with resin or the like in advance to maintain the adhesive strength of the adhesive member 17, the adhesive fixing body 16 can be used as needed. Box 1 for possible
Since the work of filling the adhesive member 17 into the sample 8 can be omitted, the work of fixing the sample A is further simplified, and the work before and after the measurement of the sample A by the X-ray diffractometer becomes easy.

Further, as shown in FIG.
A holding plate 20 larger than the bottom surface of the box 18 may be fixed to the bottom surface of the box 18 of FIG. Since the adhesive fixed body 16 has a bottom surface of 15 mm × 15 mm and a height of about 2 mm as described above, it becomes easy to handle by fixing the holding plate 20 to the box 18. Fixing to the sample holder becomes easy. At this time, the height of the adhesive fixing body 16 including the holding plate 20 is formed to be the same as the sample holding surfaces 2 and 7 so that the upper surfaces of the sample A and the sample holder for the X-ray diffraction apparatus are flush with each other. (See FIG. 11).

Further, a friction surface may be formed by providing irregularities on the side surface of the box 18 of the adhesive fixing body 16. When the friction surface is provided in this manner, friction occurs between the box body 18 and the sample holding surfaces 2 and 7, so that the adhesive fixing body 16 can be more reliably fixed. At this time, the friction surface may be formed by directly embossing the side surface of the box 18, or may be a cloth such as felt or a rubber.

The adhesive member 17 of the adhesive fixing body 16 is amorphous (for example, stick glue manufactured by Tombo Pencil Co., Ltd., product name: Pit Art Great) in order to detect X-rays diffracted by the sample A during measurement. Although it is desirable to use a non-amorphous material, it is not necessary to be amorphous when performing a blank measurement. Further, when the adhesive fixing body 16 is used repeatedly, it is desirable that the adhesive member 17 has such a property that the adhesive member 17 does not flow at room temperature but can be easily removed from the box 18 by being dissolved in a solvent or overheated. As such an adhesive member 17, in addition to the above-mentioned glue-like material including the stick glue, α-gel, photo-crosslinked PVA gel, agar, jelly, and the like can be used.

[0036]

As described above, according to the first aspect of the present invention, the sample holder mainly includes the fixed table and the movable table which are separate bodies, and holds the sample between the two tables. For,
Samples of various sizes and shapes can be held between the sample holding surfaces. Further, even when the sample is a powder, the sample can be held by using clay or the like at the portion defined by the sample holding surfaces of the fixed base and the movable base and the rod.
Therefore, since the restriction on the size of the sample is relaxed, the sample can be easily fixed to the sample holder. In the case of fixing a solid sample, since a process such as cutting is not required, a complicated operation can be omitted. In addition, since the sample can be securely fixed by the nut, the sample measurement surface does not shift during the sample measurement.

According to the second aspect of the present invention, since the tapered surface is formed on the nut, the peripheral edge of the tapered surface is press-fitted into the through hole of the movable base, so that the displacement between the rod and the through hole is eliminated. Since the movable table can be held at a stable position, the fixed table, the movable table, and the sample measurement surface can be easily coplanar.

According to the third aspect of the present invention, when the tapered surface is formed, the tapered surface is pressed into the movable table, thereby suppressing the vertical and horizontal displacement of the movable table. The sample can be reliably fixed only by placing the sample holding surface on the upper side and fixing the screw while screwing the nut.

According to the fourth aspect of the present invention, if the adhesive member is filled in a box having a side surface height equal to the height of the sample holding surface and the sample is fixed on the surface of the adhesive member, the sample A Is also a powder, it can be fixed to the sample holder.
Furthermore, since the height of the box corresponds to the height of the sample holding surface, the upper surface of the sample holder and the sample A can be made flush with each other by pressing the sample A against the adhesive member. Sample fixing work becomes easy.

[Brief description of the drawings]

FIG. 1 is a perspective view showing a structure of a sample holder for an X-ray diffraction apparatus according to one embodiment of the present invention.

FIG. 2 is a perspective view showing a structure of a nut of the sample holder shown in FIG.

FIG. 3 is a perspective view showing the sample holder shown in FIG. 1 to which a sample is fixed.

FIG. 4 is a perspective view showing a sample holder in which a friction surface is provided on a sample holding surface.

FIG. 5 is a perspective view showing a sample holder in which a locking groove is provided on a sample holding surface.

FIG. 6 is a perspective view showing a sample holder in which a locking wall is provided on a sample holding surface.

FIG. 7 is a perspective view showing a structure of a sample holder different from FIG.

FIG. 8 is a perspective view showing a structure of an adhesive fixing body used when measuring a powder sample.

FIG. 9 is a perspective view for explaining a method of fixing the adhesive fixing body to the sample holder shown in FIG.

FIG. 10 is a cross-sectional view for explaining a method for storing an adhesive fixed body.

FIG. 11 is a cross-sectional view showing a structure of an adhesive fixing body different from FIG.

FIG. 12 is a schematic view showing the structure of an X-ray diffraction device.

FIG. 13 is a perspective view showing the structure of a conventional sample holder.

FIG. 14 is a view for explaining fixing a solid sample to a conventional sample holder.

FIG. 15 is a perspective view showing a conventional sample holder to which a solid sample is fixed.

FIG. 16 is a cross-sectional view showing a structure of a sample holder having a structure different from that of the conventional sample holder shown in FIG.

FIG. 17 is a cross-sectional view showing the sample holder of FIG. 16 to which a powder sample is fixed.

FIG. 18 shows a state in which a sample is fixed by a method different from that in FIG. 17;
It is sectional drawing which shows the sample holder of No. 6.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Fixed table 2 Sample holding surface 3 Screw groove 4 Rod 5 Movable table 7 Sample holding surface 8 Nut 9 Tapered surface 16 Adhesive fixed body 17 Adhesive member 18 Box

Claims (4)

[Claims] 1. A fixed table comprising a sample holding surface and a movable table each having a sample holding surface, and a plurality of rods having screw grooves are fixed so as to protrude at a predetermined distance from the sample holding surface of the fixed table, and A sample holder for an X-ray diffractometer, comprising a nut inserted into the rod so that the sample holding surface of the movable table faces the sample holding surface of the fixed table and screwed to the rod. . 2. The sample holder for an X-ray diffraction apparatus according to claim 1, wherein an end face of said nut is formed in a tapered surface so as to press-fit said movable table. 3. A rod provided on a sample holding surface of a fixed table is inserted into the movable table so as to face the sample holding surface of the movable table, and is placed on a flat table. A method for fixing a sample, comprising mounting a sample between clamping surfaces, then screwing the nut into a rod, and tightening the nut so that the tip of a tapered surface provided on the nut is pressed into a movable table. 4. The sample fixing method according to claim 3, wherein the sample is fixed to an adhesive fixed body filled with an adhesive member in a box body having a side surface height equal to the sample holding surface. .