JPS61107145A - Specimen heating apparatus for x-ray diffraction - Google Patents

Abstract

PURPOSE:To make it possible to heat a specimen up to far high temp., by constituting at least the part, which is opposed to the front surface of a specimen, of the heater covering the entire periphery of a specimen holder from a graphite plate. CONSTITUTION:An auxiliary heater 3 comprises a thin graphite plate and is constituted of a central part 3b having a width D2 slightly larger than the width D1 of the opening part of a main heater (heating wire) 2 and both end ring shaped parts 3a each having an outer shape slightly smaller than the inner diameter of the main heater 2 and the heater for covering the entire periphery of a specimen holder 4 is formed of the main heater 2 and the auxiliary heater 3. Terminal metal fittings 4 are attached to both terminal parts of the auxiliary heater 3 by screwing or insert molding and connected to a power source along with the heating wire 2. Because a part of the heater is constituted of the graphite plate and both terminals thereof are connected to the power source to generate heat as mentioned above, the specimen 5 can be heated up to far high temp. as compared with conventional system.

Description

DETAILED DESCRIPTION OF THE INVENTION A. Field of Industrial Application The present invention relates to a sample heating device for measuring a sample while heating it in an X-ray diffraction apparatus.

- Conventional technology In this type of sample heating device, those with the front side of the sample exposed tend to have a limited heating capacity, while those with a nearly closed heating furnace and a small window have a limited X-ray scanning range. Moreover, those in which the heater wire was also provided in front of the sample had the disadvantage that the diffraction peak of the material constituting the heater appeared in the measurement results.

C. Purpose of the Invention The present invention eliminates the above-mentioned drawbacks and provides a sample heating device that has high heating capacity, does not limit the scanning range of X-rays, and does not have any effect on measurement results due to the heater material. It is something.

28 Structure of the Invention The X-ray diffraction sample heating device according to the present invention is such that at least the part facing the front surface of the sample of the heater that covers the entire circumference of the sample holder is constructed of a graphite plate connected to a power source at both ends. We focused on the fact that graphite is an electrical conductor, absorbs almost no X-rays, and has an extremely high heat resistance with a melting point of over 3000°C in vacuum (μT#-6). By covering the surface with a heater such as a graphite plate,
It has increased heating ability but does not interfere with X-ray diffraction measurements.

(LA Susu 2 4 Takub) Example FIG. 1 shows an embodiment of the present invention.

1 has a central part 37 having a width D2 slightly larger than the opening width D1 of the main heater having a cylindrical C-shaped cross section with a part of the peripheral wall opened, and an outer part 37 having a width D2 slightly larger than the inner diameter of the main heater. As shown in FIG. 2a, the main heater and the auxiliary heater 3 form a heater that covers the entire circumference of the sample holder 4. Terminal fittings are attached to both ends of the auxiliary heater 3 by screwing or insert molding, and are connected to a power source together with the heating wire 2.

As shown in FIG. 1, the X-rays enter through the graphite plate of the auxiliary heater 3, are diffracted by the sample 5, pass through the graphite plate again, and exit.

Almost no X-rays are absorbed in graphite, and the melting point of graphite is 3000°C or higher in vacuum, so the sample can be heated to around 2000°C.

Effects The sample heating device for X-ray diffraction according to the present invention is composed of the above-mentioned plate, and both ends of the plate are connected to a power source to generate heat, so it is necessary to arrange a tungsten wire, nichrome wire, etc. in front of the sample. Therefore, there is no risk of diffraction peaks of the metal that makes up the heating wire appearing in the measurement data, and since the sample is heated from the entire circumference, it is much more efficient than the conventional method where the front side is open. It has the advantage of being able to heat up to high temperatures, and even if the opening width of the main heater is made sufficiently large, there is no risk of the internal temperature cooling down, so it is possible to expand the scanning range of X-rays and increase the degree of freedom in measurement. There are advantages.

[Brief explanation of the drawing]

Fig. 1 shows an embodiment of the present invention, in which a is a partially cutaway front view, b is a plan sectional view, C is a side view, Fig. 2 a is an overall perspective view of the same as above, and b is a main part. FIG. 1... Main heater, 2... Heating wire, 3... Auxiliary heater, 4... Sample holder, 5... Sample. Agent Patent Attorney Hiroshi Tsune Figure 1 (a) 2 α a) 2 b)

Claims (1)

[Claims] 1. A sample heating device for X-ray diffraction, characterized in that at least a portion of a heater covering the entire circumference of a sample holder facing the front surface of the sample is constructed of a graphite plate.