JPH0637317Y2 - Sample holder for X-ray diffractometer - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a sample holding means in an apparatus for analyzing physical properties of a sample by X-ray diffraction.

Such an X-ray diffractometer generally rotates the sample, for example, at a constant low speed with a straight line passing through the surface of the plate-shaped sample as an axis, and from a fixed X-ray tube to an X-ray of a constant wavelength on the sample surface. Is projected, and the diffraction angle is detected by detecting the diffracted X-rays by an X-ray detector that rotates the periphery of the sample at an angular velocity twice that of the sample. However, if the sample deteriorates in the air in a short time, it must be sealed in an inert gas or housed in a vacuum. For this reason, in the past, the sample stage of the diffractometer was replaced with a closed sample chamber for observation, but precise re-adjustment was required at the time of replacement, so there was a drawback that the efficiency of observation was significantly reduced. Therefore, the present invention provides a sample holder capable of easily and quickly observing a sample as described above by mounting it on the same sample table without requiring a complicated and time-consuming adjustment operation. To do.

The sample holder of the present invention is provided with a cylindrical surface portion on the sample mount of the X-ray diffractometer and uses a bottomed cylindrical body which is hermetically fitted to the above-mentioned part through an annular packing. A sample is sealed with this cylindrical body, and a band-shaped X-ray window is formed on the circumferential side surface of the cylindrical body so as to face the sample surface, and if necessary, the bottomed cylindrical body or Provide an exhaust port on the sample mount. Therefore, by attaching the sample mount to the diffractometer and making precise adjustments,
In the case of a sample that deteriorates in air in a short time, the sample is prevented from being deteriorated by covering it with the bottomed cylindrical body and exhausting the inside, or by enclosing a dehumidifying agent together with the sample. Moreover, since the sample mounting table does not need to be replaced, it is not necessary to readjust the mounting state, and therefore, the sample easily deteriorated in the air can be efficiently observed in a short time.

FIG. 1 is a vertical sectional view of an embodiment of the present invention, FIG. 2 is a sectional view taken along the line AA in FIG. 1, and FIG. 3 is a sectional view of the same portion as FIG. 2 in an X-ray diffraction apparatus. X like this
The rotary table 1 of the line diffraction apparatus is provided with a hole 4 into which the shaft 3 of the sample mounting table 2 is fitted and fixed. On the sample mounting base 2, a cylindrical surface-shaped portion 5 whose center line is the rotation axis p of the rotary base 1 is formed, and a flat surface 6 including the axis p is formed.
And the leaf spring 7 is attached. Therefore, by attaching the mounting base 2 to the rotary base 1 and bringing the observation surface of the rectangular plate-shaped sample 8 into close contact with the plane 6 and pressing it with the spring 7 to fix it, the rotation axis p of the sample 8 becomes This sample can be mounted so that it sits on the observation surface. Further, the lid plate 10 is detachably attached by the packing 9, an arc-shaped X-ray window 11 is formed on the peripheral side surface, and the bottomed cylindrical body 13 is sealed with an X-ray transmission material 12 such as beryllium or mylar. It is provided. The open end of this cylindrical body 13 is
An annular packing 14 is formed so as to be fitted into the cylindrical surface portion 5, and an inner surface thereof is provided with an annular packing 14 and, if necessary, an exhaust port 16 having an opening / closing valve 15 is also formed. That is, when such a cylindrical body 13 is fitted into the cylindrical surface portion 5 of the sample mounting base 2, the sample 8 is accommodated in the inside thereof,
Moreover, the airtight state is maintained by the packings 9 and 14. Further, as shown in FIG. 3, the rotary table 1 is provided with a second rotary table 17 which rotates coaxially with the rotary table 1 at twice the angular velocity, and X
The X-ray tube 19 is fixed at an appropriate position while the X-ray detector 18 is attached, and the X-ray is incident on the surface of the sample 8 through the arc-shaped window 11. That is, by rotating the turntables 1 and 17 at an angular velocity of 1: 2, the sample 8
X-rays which are incident on and diffracted are always focused on the detector 18 and detected.

In the sample holder of the present invention as in the above-described embodiment, the cylindrical surface portion 5 is formed on the sample mounting base 2 and the sample 8 is formed by the bottomed cylindrical body 13 which is hermetically fitted to this portion via the packing 14. Is to be sealed. Therefore, the sample can be shielded from the outside air to prevent its deterioration and, if necessary, the exhaust port 16 is provided to exhaust the inside of the cylindrical body 13 to keep it in a vacuum state, or the inside of the cylindrical body. It is also possible to enclose an arbitrary gas, a hygroscopic agent, or the like in. Moreover, since the cylindrical body 13 is not required for a sample which is not likely to be altered, and it can be mounted on the same mounting base 2 for measurement, it is necessary to readjust the device when the sample mounting base is replaced. Not. Therefore, the X-ray diffractometer can be efficiently used for various samples and the observation efficiency is improved. Further, when the X-ray transmission material 12 is detached and used, there is an effect that the X-rays are not attenuated and the interference by the scattered X-rays can be prevented.

[Brief description of drawings]

FIG. 1 is a vertical sectional view of an embodiment of the present invention, FIG. 2 is a sectional view taken along the line AA in FIG. 1, and FIG. 3 is a plan view of an X-ray diffractometer equipped with the sample holder shown in FIGS. is there. In the figure, p is the rotation axis of the X-ray diffractometer, 8 is a sample, 2 is a sample mount, 5 is a cylindrical surface portion, 14 is an annular packing, 13 is a bottomed cylindrical body, 12 is an X-ray transparent material, 11 is an X-ray window.

Claims (1)

[Scope of utility model registration request] 1. An X-ray diffractometer, wherein a sample mounting base is formed with a cylindrical surface portion, and a center line of the cylindrical surface portion and a rotation axis of the sample mounting base are plate-shaped mounted on the sample mounting base. The sample is housed inside the bottomed cylindrical body by fitting the open end of the bottomed cylindrical body into the cylindrical surface portion through an annular packing in an airtight manner so as to ride on the analysis surface of the sample. A sample holder for an X-ray diffraction apparatus, wherein an arc-shaped X-ray window sealed with an X-ray transmitting material is formed on the peripheral side surface of a bottom cylinder.