JPH09229834A - Sample supporting device for x-ray device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To prevent a lot of frost from sticking of an amount more than the amount affecting measurement to a sample holding member which supports a sample, relating to a sample supporting device used for x-ray device which performs measurement by blowing a low temperature gas to the sample. SOLUTION: The sample supporting device is used for an x-ray device wherein a sample S is irradiated with the x-ray from an x-ray source F, and the x-ray coming out of the sample S is detected with an x-ray detector 4. The sample S is fixed to and supported by the upper end of a sample supporting member 9 which is formed by applying the outside periphery surface of a glass rod 11 with a silver paste 12 of high thermal conductivity. When coolant gas G1 and G2 blowing off from a nozzle 15 is blown to the sample S so that the temperature of the sample S is kept at low, thanks to the function of the thermal conductivity of the silver paste 12, large frost is prevented from growing such part of the sample supporting member 9 as hit by coolant gas.

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to a sample support device used for supporting a sample in an X-ray apparatus.

[0002]

2. Description of the Related Art An X-ray apparatus for analyzing a crystal structure of a sample using X-ray is widely known. In this X-ray apparatus, it may be desired to measure the structural change of the sample under a low temperature condition. In this case, conventionally, as shown in FIG.
While holding the sample S in a low temperature state by blowing the low temperature gas G onto the sample S supported by 1, the sample S is irradiated with the X-rays emitted from the X-ray source F, and the sample S diffracts and reflects the light. The X-ray is detected by the X-ray detector 52.

In this conventional sample support device, the sample S
The reason why glass is used instead of metal as a rod material for supporting is because of the following reasons. That is, when a metal is used, when irradiating the sample with X-rays, the X-rays also hit the metal rod to generate scattered X-rays, and the scattered X-rays are transmitted to the X-ray detector 52 as noise components. This is because it will be detected.

[0004]

However, in the above-described conventional sample support device, when the sample is cooled to a low temperature for measurement, frost is formed on the outer peripheral surface of the glass rod supporting the sample, particularly on the outer edge portion of the refrigerant gas. Z attaches and grows further. When the amount of adhered frost Z exceeds a predetermined amount, X-rays generate the frost Z.
On the other hand, scattered X-rays are generated, and as a result, the measurement accuracy may deteriorate.

The present invention has been made in view of the above problems, and in a sample support device used in an X-ray apparatus for measuring a sample by spraying a low temperature gas, the sample support for supporting the sample The purpose is to prevent a large amount of frost from adhering to the member from damaging the measurement.

[0006]

In order to achieve the above object, a sample supporting device according to the present invention comprises a sample supporting member for supporting a sample and a sample supporting member which is laminated on an outer peripheral surface of the sample supporting member. Also has a coating material having a high thermal conductivity. According to this sample support device, a small amount of frost adheres to the outer peripheral surface of the sample support member, but it does not grow much and the generation of scattered X-rays also disappears. As a result, highly accurate X-ray measurement results are obtained. Can be obtained. It is considered that this is because the thermal gradient generated in the sample support member becomes gentle by the action of the coating material.

The sample support member is formed in an arbitrary shape capable of supporting the sample, and can be formed of, for example, a rod or a tube. When the rod is used, the sample is fixed to the tip of the rod. In the case of a pipe material, the sample is stored inside the pipe. The material for the sample support member is preferably a material that does not generate scattered X-rays when irradiated with X-rays, such as glass.

Various treatment methods for laminating the coating material on the outer peripheral surface of the sample support member are conceivable and are not limited to specific methods. For example, a method of applying with a coating tool such as a brush, a method of applying by spraying, a method of immersing the sample support member in a tank storing the coating material, and a method of applying a thin layer of the coating material to the outer peripheral surface of the sample support member. Any treatment method can be used as long as it can be adhered to and fixed to. As the coating material, metal paste, paint containing metal, or the like can be used. The metal paste may be silver paste or the like.

[0009]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS FIG. 1 shows an embodiment of an X-ray apparatus using a sample support device according to the present invention. This X
The X-ray device has an X-ray source F installed on one side of the sample support device 3 and an X-ray film 4 as an X-ray detector installed on the other side of the sample support device 3. . The X-ray film 4 is a two-dimensional X-ray detector that can detect X-rays in a plane, but instead of this, a one-dimensional X-ray detector that detects X-rays in a dot shape is installed and the X-ray film is used as an X-ray film. It can be moved in the line diffraction direction.

The sample support device 3 includes a goniometer 5 and a goniometer head 6 mounted on the goniometer 5.
And a sample unit 7 attached to the goniometer head 6. The goniometer head 6 includes a Y stage 13y arranged on the goniometer 5, an X stage 13x mounted on the Y stage 13y, and a Y direction arc stage 14y mounted on the X stage 13x. , And an X-direction arc stage 14x mounted on the Y-direction arc stage 14y.

The Y stage 13y supports the X stage 13x mounted on the Y stage 13y so as to be movable in parallel in the direction perpendicular to the plane of the drawing. As indicated by an arrow A, the X stage 13x supports a Y-direction arc stage 14y mounted on the X-stage 13x so that the Y-direction arc stage 14y can move in parallel in the left-right direction of the drawing. The Y-direction arc stage 14y is an X-direction arc stage 1 mounted on it.
4x is supported so that it can freely perform an arc motion, that is, an arc motion centered on the sample S in the direction perpendicular to the plane of the drawing. Then, the X-direction arc stage 14x supports the sample unit 7 mounted on the sample unit 7 so that the sample unit 7 can be freely arc-moved in the left-right direction of the drawing sheet around the sample S as shown by an arrow B.

By the function of the goniometer head 6 configured as described above, the sample S can be moved in the plane by parallel movement in the two orthogonal directions, and further, the X-ray beam can be moved by the arc movement in the two orthogonal directions. The azimuth can be changed. The goniometer head 6 used in the present embodiment uses the sample S in the plane and orthogonally 2
Although it is a type that can move in the direction of the arc, various types of goniometer heads, such as a type that can move only in a plane or a type that can perform only arc movement, can be used.

As shown in FIG. 2, the sample unit 7 includes a metal rod 8, a rod-shaped sample support member 9 fixed to the upper end of the metal rod 8 by brazing, and the sample support member 9. The sample S is bonded to the upper end with grease, resin, or the like. The lower end of the metal rod 8 is fixed to the upper end of the X-direction arc stage 14x of the goniometer head 6 with an adhesive or with a screw. The sample support member 9 is formed by applying a coating material 12 having a higher thermal conductivity than glass, for example, a silver paste, to the outer peripheral surface of the glass rod 11.

Returning to FIG. 1, a gas blowing nozzle 15 is arranged near the sample S. As shown in FIG. 2, the gas spray nozzle 15 comprises an inner pipe 15a and an outer pipe 15b.
It is composed of a heavy pipe, and as shown in FIG. 1, the gas spray nozzle 15 is connected to a low temperature gas supply device 16. The low-temperature gas supply device 16 sends a refrigerant gas such as low-temperature air or low-temperature nitrogen gas to the gas spray nozzle 15 at high pressure, and the supplied gas is sprayed from the nozzle 15 to the sample S.

As shown in FIG. 2, the main gas flow G1 is injected from the inner pipe 15a, and the sample S is mainly cooled by this. Then, the gas auxiliary flow G2 is injected from the outer pipe 15b, thereby forming a gas curtain around the gas main flow G1. The gas curtain enhances the cooling efficiency of the sample S. The gas curtain is required when the sample S is set to a very low temperature,
When setting a relatively high temperature, for example, -20 ° C or higher, the gas curtain is not necessary.

Returning to FIG. 1, the goniometer 5 is a sample S.
Is continuously or intermittently rotated around a central axis ω at a predetermined angular velocity, so-called θ rotation. The goniometer 5 can be configured by, for example, a pulse motor as a power source and a power transmission system that transmits the rotation of the pulse motor to the goniometer head 6. The power transmission system can be composed of, for example, a worm and a worm gear that mesh with each other.

Since the X-ray apparatus and the sample support apparatus of this embodiment are constructed as described above, first, in FIG. 1, the goniometer head 6 is adjusted to accurately measure the sample S in the X-ray direction.
Position on the line optical axis. After that, in FIG. 2, the refrigerant gas is continuously jetted from the gas spray nozzle 15 so that the sample S
To the desired low temperature and hold that temperature. And
In FIG. 1, an X-ray is emitted from an X-ray source F, the X-ray is processed by an X-ray filter, a monochromator, or the like as necessary, and then the sample S is irradiated.

When the X-ray diffraction condition is satisfied between the irradiated X-ray and the crystal lattice plane of the sample S, X is generated at the crystal lattice plane.
The rays are diffracted and the diffracted X-rays reach the X-ray film 4 to expose it, and as a result, an X-ray image corresponding to the diffracted X-rays is recorded on the X-ray film 4. By observing this X-ray image, the crystal structure or the like of the sample S is analyzed.

In the present embodiment, as shown in FIG. 2, the sample support member 9 for supporting the sample S is composed of a glass rod 11 and a coating material 12 for coating the glass rod 11. A silver paste with high conductivity was used. Therefore, when the refrigerant gases G1 and G2 are blown to the sample support member 9, a small amount of frost may be formed on the sample support member 9, but the frost does not grow greatly. Therefore, when the sample S is irradiated with X-rays,
It is possible to perform highly accurate measurement with less generation of scattered X-rays.

FIG. 3 shows another embodiment of the sample support device according to the present invention. This embodiment differs from the embodiment shown in FIG. 2 in that the sample support member 19 is replaced by the glass tube 2
1 and the coating material 12 applied to the outer peripheral surface of the glass tube 21. In this embodiment,
The sample S and the mother liquor 17 are stored inside the glass tube 21, and then the opening of the glass tube 21 is sealed by brazing R or the like. The lower end of the glass tube 21 is fixed to the upper end of the metal rod 8 by brazing or the like. The mother liquor 17 is a crystallization solvent and prevents the sample S from drying or the like. The sample S is
Glass tube with mother liquor, grease, epoxy resin, etc. 2
It is fixed to the inner wall of 1.

A silver paste is also used as the coating material 12, and the silver paste is applied to the outer peripheral surface of the glass tube 21. However, since the sample S is irradiated with a sufficient amount of X-rays, the silver paste is not applied to the glass tube wall around the sample S corresponding to the X-ray passage. Even in the case of this embodiment, the gas spray nozzle 15 is provided by providing the coating material 12.
When the refrigerant gases G1 and G2 are blown from the above, it is possible to prevent a large amount of frost from growing on the portion of the sample support member 19 where the refrigerant gas is blown, particularly the outer edge portion thereof.

The present invention has been described above with reference to the preferred embodiments, but the present invention is not limited to these embodiments, and various modifications can be made within the scope of the invention described in the claims. . For example, the sample support device of the present invention is
The present invention can be applied to an X-ray device having any structure other than the X-ray device having the structure shown in FIG. Further, as the coating material 12, an appropriate metal paste other than silver paste can be used,
In addition, a paint containing metal can be used. Further, the covering member 12 can be laminated on the outer peripheral surface of a glass rod, a glass tube or the like by using any film forming method other than coating.
It is generally considered that the base material of the sample support member is formed of glass, but it is of course possible to form it by using an appropriate material other than that.

[0023]

According to the sample support device of the present invention, since the coating member having a high thermal conductivity is laminated on the outer peripheral surface of the sample support member, that is, adhered in close contact with the sample support member, the refrigerant gas is blown to the sample support member. However, on the surface of the sample support member, X
It is possible to prevent a large amount of frost from adhering to the line measurement which is harmful.

[0024]

[Brief description of drawings]

FIG. 1 is a front view showing an embodiment of an X-ray apparatus using a sample support device according to the present invention.

FIG. 2 is a perspective view showing a main part of an embodiment of a sample support device.

FIG. 3 is a perspective view showing a main part of another embodiment of the sample support device.

FIG. 4 is a perspective view showing a main part of an example of a conventional sample support device.

[Explanation of symbols]

 3 sample support device 4 X-ray film 5 goniometer 6 goniometer head 7 sample unit 8 metal rod 9 sample support member 11 glass rod 12 coating material 15 refrigerant gas spray nozzle 19 sample support member 21 glass tube F X-ray source G1 refrigerant gas mainstream G2 Refrigerant gas sidestream S Sample Z Frost

Claims (7)

[Claims] 1. A sample supporting device for use in an X-ray device for irradiating a sample with X-rays and detecting the X-rays emitted from the sample by an X-ray detecting means, the sample supporting member supporting the sample, A sample support device for an X-ray apparatus, comprising: a coating material laminated on the outer peripheral surface of the support member and having a higher thermal conductivity than the sample support member. 2. The sample support device for an X-ray apparatus according to claim 1, further comprising a low temperature gas spraying unit for spraying a low temperature gas toward the sample. 3. The sample support device for an X-ray apparatus according to claim 1, wherein the sample support member is a rod. 4. The sample support device for an X-ray apparatus according to claim 1, wherein the sample support member is a tube material. 5. The sample support device for an X-ray apparatus according to claim 1, wherein the sample support member is made of glass.
Line device sample support device. 6. The sample support device for an X-ray apparatus according to claim 1, wherein the coating material is a metal paste. . 7. The sample support device for an X-ray apparatus according to claim 6, wherein the coating material is silver paste.