JPS6363953A - Specimen support device for diffracted x-ray observation - Google Patents

Abstract

PURPOSE:To perform positioning simply, rapidly and certainly, by constituting a support member, wherein the hollow specimen introducing pipe connected to the opening part of a glass sphere and the glass sphere are integrally formed, of an insert handle and a head for fixing a specimen to the leading end of said handle. CONSTITUTION:In using this specimen support device, a specimen 1 to be heated is accurately fixed to the head 3a made fine of a support member 3 by a heat resistant adhesive and, next, the spherical part of a heat resistant glass sphere 2 is held downward in a vertical state to insert the aforementioned support member 3. When the support member 3 is inserted up to a position where the shoulder parts 2c, 3c of both jigs contact with each other, the insert handle 3b of the support member 3 becomes the state engaged with the specimen introducing pipe 2b of the heat resistant glass sphere 2 and, when planning is preliminarily performed so that the specimen 1 to be heated is positioned at the central part of the heat resistant glass sphere 2 at that position, centering operation is automatically performed and positional shift is prevented.

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention is applicable to laser heating and X-ray diffraction, which are necessary for tracking the behavior of crystal lattices of single crystal or polycrystalline materials at high temperatures and for searching for new materials. , relates to a sample support for diffraction X-ray observation that holds a sample.

[Prior Art] While heating a solid sample such as a single crystal or polycrystalline material to a high temperature, changes in crystallinity and crystal lattice are measured in situ (in 5 itu) using physical evaluation methods such as X-ray diffraction.
The observation method is already known.

The heating methods used in this case include electrical resistance heating, gas burner heating, concentrated infrared heating, and electron beam heating, but all of these tend to require large-scale equipment and cannot be combined with an X-ray diffraction device. In some cases, the spatial freedom of the device is restricted, which limits the collection of high-temperature data that is readily available, making it difficult to make complete comparisons with room-temperature data. Therefore, recently developed Nd:
A method of guiding an infrared laser beam such as YAG to the vicinity of a sample using a glass fiber, and then focusing and heating the sample using an optical lens was proposed in the Proceedings of the International Symposium on Ceramic Components. Four Order Engine J (Pro
ceedings of International
5ytposiulIlon Ceramic Com
components for Engine).

It was proposed on page 519 of the 1983 Japanese edition, and has attracted attention as a method that significantly expands the degree of freedom in data collection at high temperatures.

[Problems to be Solved by the Invention] In the above proposal, if it is necessary to heat the sample in vacuum or in an inert gas, the sample to be heated 11 is heated as shown in FIG. 2(a). Heat-resistant glass sphere 12 in the shape of a miniature light bulb
must be enclosed in. Note that the material of this heat-resistant glass sphere 12 shall be transparent to the X-rays and laser beams used. During the experiment, the heated area of the sample and the irradiated area of the X-ray must be the same, otherwise the crystallographic orientation method during X-ray diffraction, the laser
Since it is difficult to position the sample 11 to produce the maximum effect on the beam, it is essential to correctly position the sample 11 to be heated at the center of the heat-resistant glass sphere 12 (centering). Positioning of the heated sample 11 is as follows:
This is done using a rod-shaped support member 13 as shown in FIG. 2(b). Conventionally, after the sample 11 to be heated is adhered to a heat-resistant support member 134, the heat-resistant The support member 13 shall be enclosed within the glass sphere 12, and at that time, the support member 13 is
Since the method used was to tighten one end of the center, the centering was inconsistent, requiring a high level of skill, and usually required multiple trials and errors before a good result could be obtained.

The present invention has been made in order to solve these conventional problems, and provides a sample support for diffraction X-ray observation that allows the positioning of a heated sample to be performed simply, quickly, and reliably. With the goal.

[Means for Solving the Problems] The present invention comprises a heat-resistant glass sphere that is transparent to laser light and X-rays and can be sealed against atmospheric gas, and a sample placed at a predetermined position inside the glass sphere. A sample support for diffraction X-ray observation comprising a support member to be arranged, the glass sphere is integrally formed with a hollow sample introduction tube connected to an opening of a glass sphere, and the support member is connected to the sample introduction tube. This is a sample support for diffraction X-ray observation, characterized by comprising an insertion handle whose outer dimensions and shape correspond to the inner dimensions of the handle, and a head for fixing a sample to the tip of the insertion handle.

[Function] A sample introduction tube is attached to the heat-resistant glass sphere, an insertion handle is formed on the support member, and the insertion handle is fitted to the sample introduction tube by matching the shape and dimensions of the sample introduction tube and the insertion handle. The sample to be heated, which is mounted on the head of the support member, is positioned at a predetermined center within the heat-resistant glass sphere by simply doing so.

[Example] Hereinafter, one embodiment of the present invention will be described in detail with reference to the drawings.

FIG. 1 is a longitudinal sectional view showing a sample support for diffraction X-ray observation according to an embodiment of the present invention, in which FIG. 1A shows a glass sphere and FIG. 1B shows a support member. In both figures, the sample support device is composed of a miniature light bulb-shaped heat-resistant glass sphere 2 that encloses the heated sample 1 and a rod-shaped support member 3 that holds the heated sample 1. opening 2
A hollow sample introduction tube 2b is integrally formed in a, and on the other hand,
The support member 3 consists of a head 3a that fixes the sample to be heated 1 at a narrow tip, and an insertion handle 3b whose outer dimensions and shape correspond to the inner dimensions of the sample introduction tube 2b. In this embodiment, the shape of the sample introduction tube 2b and the insertion handle 3b is such that shoulder portions 2C and 3C are formed in the middle in the longitudinal direction, being thinner on the spherical side and thicker on the insertion side, and for changing the diameter of the jig.

When using this sample support device, the heated sample 1 is properly fixed to the thin head 3a of the support member 3 with heat-resistant adhesive, and then the spherical part of the heat-resistant glass sphere 2 is held vertically downward. Then, the support member 3 is inserted. When inserted to the position where the shoulders 2C and 3C of both vessels are in contact, the insertion handle 3b of the support member 3 is inserted into the sample introduction tube 2b of the heat-resistant glass sphere 2.
If the heating sample 1 is designed in advance to be positioned at the center of the heat-resistant glass sphere 2 at that position, it will be automatically centered and the position will be fixed. Don't go crazy. When the sample to be heated 1 is positioned, the sample introduction tube 2b and the insertion handle 3b are finally sealed at the desired position, and the sample is cut to an appropriate length as shown in FIG. 1(C). . Sealing can be done using a sealant or a tightening method, and as long as they are fitted together, the positioning will not be disturbed.

In this way, the sample to be heated is mounted in the sample supporter for diffraction X-ray observation. As a heated sample, s
In order to investigate the thermal behavior near the melting point or sublimation point of single crystal samples such as r, s; However, even if exposed to high temperatures, the sample surface will not be oxidized.
The desired high temperature data were obtained.

[Effects of the Invention] As explained above, according to the present invention, a sample supporter for diffraction X-ray observation is provided that allows positioning of a heated sample, which has been difficult in the past, to be performed easily, quickly and reliably. This has a great effect in contributing to the facilitation of heating observation methods.

[Brief explanation of the drawing]

FIG. 1 is a longitudinal sectional view showing an embodiment of the present invention, and FIG. 2 is a longitudinal sectional view showing a conventional sample supporter for diffraction X-ray observation. 1.11... Sample to be heated 2, 12... Heat-resistant glass sphere 2a... Opening part 2b... Sample introduction tube 2c, 3c... Shoulder part 3, 13... Support member 3a...・Head 3b...Insertion handle 12
a... Root part Fig. 1 (b) (C)!

Claims (1)

[Claims] A sample support for diffraction X-ray observation consisting of a heat-resistant glass sphere that is transparent to laser beams and X-rays and can be sealed against atmospheric gas, and a support member that places the sample at a predetermined position inside the glass sphere. An insertion handle in which a hollow sample introduction tube connected to an opening of a glass sphere and the glass sphere are integrally formed, and a support member has an outer size and shape corresponding to the inner dimensions of the sample introduction tube. A sample support for diffraction X-ray observation, comprising: a head for fixing a sample to the tip thereof;