JPH05307012A - Airtight specimen holder for x-ray diffraction device - Google Patents

Abstract

PURPOSE:To hold a micro-specimen in the desired atmosphere at a specified position of an X-ray diffraction device where an airtight vessel for specimen can not be located on the device body being obstructed by a swinging mechanism. CONSTITUTION:A specimen encapsulating part 2 made of a transparent material is formed at a part of a holder body 1, and in a separately provided airtight vessel such as a glow box, a specimen S is inserted in this specimen encapsulating part 2, which is then shut by a shutting member 3. Thereby, the part 2 is held in atmosphere similar to the inside of the airtight vessel. Mounting on an X-ray diffraction device is conducted while the operator watches the specimen S in this part 2 with a microscope.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an airtight sample holder used in an X-ray diffractometer equipped with a movable sample table, and more particularly to an airtight sample holder for arranging a minute sample at the swing center of the sample table.

[0002]

2. Description of the Related Art As shown in FIG. 3, an X-ray diffractometer for analyzing the crystal structure of a substance by utilizing the X-ray diffraction phenomenon
There is a structure in which the sample table 10 swings around a support shaft 11. The schematic configuration of the X-ray diffractometer shown in FIG.
The sample fixed to the tip of the sample table 10 is irradiated with X-rays emitted from the X-ray tube 12 through the collimator 13. Since the X-rays irradiated on the sample are diffracted in a specific direction according to the crystal structure of the sample, the diffracted X-rays are detected by the detector 14, and the X-ray of the sample is detected based on the relationship between the detected angle and the irradiation angle. The crystal structure etc. can be analyzed.

The sample table 10 swings about a support shaft 11 in order to adjust the irradiation angle of X-rays on the sample, is rotatable about a support shaft 15, and also swings about a support shaft 16. It is free to move.

These swing and rotation center lines intersect at one point 0, and the intersection (hereinafter referred to as the center of movement) 0 intersects the path of the X-rays emitted from the collimator 13. The sample is placed on the center of movement 0. However, since the sample to be inspected by this X-ray diffractometer is a microcrystalline material, it is difficult to position it with the naked eye. Therefore, the apparatus is provided with a microscope 17 for positioning the sample.

[0005]

Conventionally, the above-mentioned X-ray diffractometer was limited in its use to the structural analysis of substances in the atmosphere. However, for example, when the sample to be inspected is a substance that may react with oxygen in the atmosphere and is oxidized in a short time, it is difficult to analyze the structure of the substance in a normal state. On the contrary, there is a case where it is desired to acquire the structural change data of the sample under various atmospheres.
In the line diffractometer, it was not possible to obtain such data because the atmosphere around the sample could not be set arbitrarily. However, in the X-ray diffractometer of the type that does not have a swinging mechanism of the sample stage, there is conventionally known a structure in which the sample stage is arranged in a closed container and the inside of the container can be set to a desired atmosphere. Was there. However, in the X-ray diffractometer of the type having the swing mechanism of the sample stage as shown in FIG. 3, the swing mechanism interferes with the installation of the closed container, so the atmosphere setting structure around the sample by the closed container is adopted. Was difficult.

The present invention has been made based on such conventional circumstances, and enables analysis by an X-ray diffractometer equipped with a movable sample stage in a state where the sample is placed in an arbitrary atmosphere. It is intended to provide an airtight sample holder.

[0007]

In order to achieve the above object, the present invention provides an airtight sample which is mounted on a movable sample stage in an X-ray diffractometer and a minute sample is arranged at the center of movement of the sample stage. A holder, which is configured to include a holder main body that can be mounted on the sample base, a sample encapsulating portion made of a transparent material provided in a part of the holder main body, and a closing member that seals the sample encapsulating portion. ..

[0008]

According to the present invention having the above-described structure, the sample is placed in the sample enclosing portion in a closed container such as a glow box which is set to a desired atmosphere in advance, and the sample enclosing portion is closed by the closing member. The inside of the sample-sealed portion thus sealed is the same as the internal atmosphere of the sealed container. Then, the holder main body is mounted on the sample table, and the sample is positioned at the moving center of the sample table while observing the sample with a microscope through the peripheral wall of the transparent sample enclosing part.

[0009]

DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention will be described below with reference to the drawings. FIG. 1 is a sectional front view showing a state in which an airtight sample holder according to an example of the present invention is mounted on a sample stage in an X-ray diffraction apparatus. In addition, FIGS.
[Fig. 3] is a sectional front view showing each member constituting the airtight sample holder. The present example shows a preferred example as an airtight sample holder to be mounted on the sample stage 10 in the X-ray diffraction apparatus shown in FIG.

As shown in these figures, the airtight sample holder of this embodiment is mainly composed of a holder body 1, a sample enclosing portion 2 and a closing member 3. Holder body 1
Is made of a metal material such as stainless steel and has a base peripheral wall 1a.
Is processed to a size that can be fitted into the holder mounting portion 10a of the sample table 10. Further, the holder body 1 has a hollow portion 1b into which the closing member 3 is fitted, and an internal thread portion 1c is formed on the inner wall of the hollow portion 1b over a certain length. At the center of the tip of the holder body 1, a through hole 1d for joining the sample enclosure 2 is formed.

The sample enclosing portion 2 is formed in a cylindrical shape with the tip closed, and the base end is fitted into the through hole 1d of the holder body 1,
It is fixed with an adhesive or the like. Therefore, the base end opening of the sample enclosure 2 communicates with the hollow portion 1b of the holder body 1. The sample enclosing section 2 is formed of a transparent material such as glass, quartz glass, or plastic so that the sample enclosed inside can be observed by an external microscope. Also, the thickness of the peripheral wall reduces absorption of X-rays,
It is formed as thin as possible (for example, about 0.01 mm).

Similar to the holder body 1, the closing member 3 is made of a metal material such as stainless steel, and the peripheral wall 3a is processed to a size that allows it to be fitted into the hollow portion 1b of the holder body 1.
A male screw portion 3b screwed into the female screw portion 1c of the holder body 1 is formed at the base portion of the peripheral wall 3a, and further, an O-ring 4 is attached to the base end in order to realize a completely sealed state. Further, a sample holding member 5 for holding the sample and disposing the sample in the sample enclosing section 2 is provided at the center of the tip of the closing member 3. The sample holding member 5 is made of a thin glass rod or the like, and its base end is embedded in the central portion of the tip of the closing member 3. Then, the sample S can be held at the tip.

Next, a method of using the airtight sample holder having the above structure will be described. First, an airtight container such as a glow box is separately prepared, and the inside of the airtight container is set to a desired atmosphere in advance. The sample S of the substance to be analyzed is fixed to the tip of the sample holding member 5, and grease is applied to the peripheral wall of the closing member 3 in order to enhance the hermeticity. Note that the work of fixing these samples and applying grease may be performed in an airtight container if necessary.

Next, each component of the airtight sample holder is carried into the airtight container. In the airtight container, the tip of the sample holding member 5 is inserted into the hollow portion 1b of the holder body 1, the peripheral wall 3a of the closing member 3 is then fitted into the hollow portion 1b, and the male and female screw portions 1c and 3b are screwed together. To do. By this operation, the sample S fixed to the tip of the sample holding member 5 is placed in the sample enclosing section 2. Further, the inside of the sample enclosing unit 2 is kept in the same atmosphere as the inside of the airtight container, and is closed by the closing member 3.

After the above-mentioned work is completed, the airtight sample holder is taken out of the airtight container, and the holder mounting portion 10a of the sample table 10 in the X-ray diffraction apparatus is attached to the base peripheral wall 1 of the holder body 1.
Insert a. Further, the sample S in the sample enclosure 2 is positioned at the center of movement 0 using the microscope 17.

The airtight sample holder mounted on the X-ray diffractometer in this manner holds the sample S in the sample enclosure 2 which is kept in a desired atmosphere. Therefore, for example, in the case of a sample that easily oxidizes, the sample in the normal state can be analyzed by setting the inside of the sample enclosure 2 in a deoxidized atmosphere. In addition, structural change data of the sample under various atmospheres can be easily obtained. Further, since the inside of the sample enclosing section 2 is hermetically closed, it is effective in preventing moisture, and in addition, it is effective in preventing scattering of the sample to the surroundings.

The present invention is not limited to the above-described embodiment, and various modifications and applications are possible within the scope of the invention. For example, the X-ray diffractometer to which the airtight sample holder of the present invention can be applied is not limited to the structure shown in FIG. 3, but various X-ray diffractometers equipped with a sample stage moving mechanism and inspecting a minute sample. Of course, a line diffraction device is applicable. In addition, the holder body, sample enclosure,
It goes without saying that the shape, material, etc. of the closing member can be changed as needed.

[0018]

As described above, according to the airtight sample holder of the present invention, it is possible to realize a simple structure by equipping the movable sample stage and mounting it on the X-ray diffraction device for analyzing a minute sample. This has the effect of enabling structural analysis of a sample under an arbitrary atmosphere.

[Brief description of drawings]

FIG. 1 illustrates an airtight sample holder according to an embodiment of the present invention,
It is a cross-sectional front view which shows the state mounted in the sample stand in a line diffraction apparatus.

2 (a) and 2 (b) are cross-sectional front views showing respective members constituting the airtight sample holder.

FIG. 3 is a perspective view showing a configuration example of an X-ray diffractometer to which the airtight sample holder of the present invention is attached.

[Explanation of symbols]

 1 Holder Main Body 2 Sample Encapsulation Part 3 Closing Member 4 0 Ring 5 Sample Holding Member 10 Sample Stand 12 X-ray Tube 13 Collimator 14 Detector 17 Microscope S Sample

Claims (1)

[Claims] 1. An airtight sample holder, which is mounted on a movable sample stage in an X-ray diffraction apparatus, and places a minute sample at the center of movement of the sample stage, the holder body being mountable on the sample stage, An airtight sample holder for an X-ray diffractometer, comprising: a sample enclosing part made of a transparent material provided in a part of the holder body; and a closing member for sealing the sample enclosing part.