JPS61124853A - Apparatus for measuring lattice constant - Google Patents

Abstract

PURPOSE:To make it possible to measure the lattice constant of a monocrystal with high accuracy, by limiting the irradiation area of X-rays to a specimen crystal by a rectangular slit and minimizing the measured area to enhance the repeated accuracy of measurement. CONSTITUTION:Incident X-ray beam 3 is controlled so as to irradiate both crystals of a standard specimen 10 and a measuring specimen. At this time, in order to measure an area as small as possible in the measuring specimen 11 and to hold parallelization of incident X-ray beam 3, a slit 7 is inserted between a monochrometer and specimen crystals 10, 11. The slit 7 has a rectangular slot 15, for example, having a dimension of 0.5X15mm and X-ray beam 3 passes through said slot 15. X-ray beam abcd limited by the slot 15 of the slit and the standard specimen is formed on the measuring specimen 11. When the irradiation area of the beam is made small, a slit insert mechanism 7 is moved to the direction shown by the arrow S.

Description

[Detailed Description of the Invention] [Field of Application of the Invention] The present invention relates to an apparatus for measuring the lattice constant of a single crystal material. The present invention relates to a device that measures a lattice constant with high precision by having a mechanism for accurately adjusting it.

[Background of the invention]

As described in Japanese Patent Laid-open No. 49-3677, a conventional device has a slit that divides the X-ray beam generated from the X-ray source into two directions, and the lattice constant measuring device has a slit that divides the X-ray beam generated from the X-ray source into two directions. A monochromator that reflects each of the X-ray beams divided into directions, and a plurality of single crystals fixed on the same rotary table, each of which is reflected by the monochromator, is set under diffraction conditions. It was a device for measuring the lattice constant yield of single crystals arranged so as to satisfy the following conditions. However, the above description does not say anything about the method of limiting the X-ray beam irradiated to the sample crystal, which is an important part of this measuring device. Therefore, if you use the slit insertion mechanism of the present invention, you can always accurately control the X-ray irradiation area.
It is possible to carry out high-precision measurements with good reproducibility.

[Purpose of the invention]

An object of the present invention is to use a lattice constant measuring device to limit the irradiation area of an X-ray beam on a sample crystal using a rectangular slit, minimize the measurement area, and improve the repeatability of measurements. The constant is Δd/d 10
An object of the present invention is to provide a lattice constant measuring device capable of measuring with high accuracy of -6 to 10-8.

[Summary of the invention]

The feature of the present invention is that the lattice constant measuring device uses a horizontally long rectangular slit and moves the slit in parallel in the horizontal direction to limit the X-ray irradiation area of the measurement sample made with the standard sample. Ta.

With this mechanism, even if the measurement sample is rotated by about 180 degrees, the same measurement area can be easily created. This improves the measurement accuracy of lattice constants.

[Embodiments of the invention]

An embodiment of the present invention will be explained below with reference to FIG. 1st
The figure shows an outline of the lattice parameter measuring device. 1 is an X-ray source. X-rays generated from an X-ray source 1 are split by a slit 2 into X-ray beams 3.4.

The X-ray beam 3 is monochromated by a monochromator 5 and irradiated onto a standard sample 10 and a measurement sample 11 fixed on a rotating table 9. At this time, the irradiation area is limited by the slit 7.

The incident X-ray beam 3 rotates smoothly in 12 directions, causing diffraction in a direction that satisfies the diffraction conditions, and enters the counter 13 where it is measured as a diffraction peak from the standard sample 10 and a diffraction peak from the measurement sample 11. Ru. The difference in Black angle between both diffraction peaks at this time is measured as ΔS.

Diffraction by the X-ray beam 4 rotates the sample stage 9 by about 180 degrees, and like the X-ray beam 3, the diffraction line is measured by the counter 14, and the angular difference at this time is defined as ΔS'.

Therefore, the amount of change in the lattice constant can be determined using equation (1).

Here, Δd==d, -do, d is the lattice spacing of the measurement sample, and do is the lattice spacing of the standard sample 10.

In addition, θ0 is the standard sample 10 with respect to the wavelength λ0 of the incident X-ray.
is Black's angle.

The lattice constant can be determined using the above measurement method, but the important thing in this method is that X4g! In the measurement of the beam 3 and the X-ray beam 4, the positions on the measurement sample where the X-ray beam is restricted by the slits 7 and 8 must be the same.

FIG. 2 shows an embodiment of the slit insertion mechanism of the device of the present invention. It is assumed that FIG. 2 is based on the Xa beam 3 in FIG. 1. Incidence X#! It is assumed that the beam 3 is adjusted in advance so as to irradiate both the crystals of the standard sample 10 and the measurement sample 11. At this time, a slit 7 is inserted between the monochromator 5 and the sample crystal 10, 11 in order to measure the smallest possible area of the measurement sample 11 and to maintain parallelism of the incident X-ray beam 3. For example, the slit 7 has a diameter of 0.5 mm at its center.
It has a rectangular hole 15 of x15wm, through which the X-ray beam 3 passes. An X-ray beam abed limited by the slit hole 15 and the standard sample 10 is formed on the measurement sample 11 . If the irradiation area of this beam is to be made smaller, this can be done by moving the slit insertion mechanism 7 in the direction of arrow S.

In the explanation of Fig. 1, when measuring the lattice constant, the measurement is performed using the X-ray beam 4, that is, the sample stage 9 is rotated approximately 180 degrees. However, if the irradiation position of the X-ray beam is different between the two, the measurement accuracy will be directly affected. Affect.

Therefore, this purpose can be achieved by using slits 7 and 8 of the same specification as shown in FIG. 1, monitoring the X-ray intensity with counters 13 and 14, and adjusting the intensity to be the same.

FIG. 3(a) schematically shows the X-ray irradiation position in the measurement using the XIW beam 3 and the detection situation of the diffraction line 16. FIG. 3(b) shows the X-ray beam 4 and the diffraction lines 17 at that time. As is clear from both figures, measurement sample 1 produces diffraction lines that reach counters 13 and 14.
1 area 1.12 and 1, /1. / are equal. Therefore,
By using the slit insertion mechanism of the present invention, the size of the measurement area on the measurement sample 11 can be easily and arbitrarily selected, and at the same time, the X-ray irradiation position can be accurately set.

〔Effect of the invention〕

According to the present invention, the X-ray irradiation area (analysis area) of the measurement sample can be arbitrarily and easily selected, and at the same time, there is no difference in the irradiation area due to a difference in the incident direction of the X-rays. The lattice constant measurement according to the present invention is 10-6 in Δd/d.
~10-@ High precision temperature measurement Figure 1 is a schematic plan view of the lattice constant measuring device, Figure 2 is a perspective view showing one embodiment of the slit insertion mechanism of the present invention, and Figure 3 is X-ray irradiation by slit insertion. FIG. 3 is a diagram showing the relationship between portions and diffraction line information.

1... X-ray source, 2... Slit, 5, 6... Monochromator 17, 8... Slit insertion mechanism, 9...
・Sample stand, 10... Standard sample, 11... Measurement sample,
13.14...Counter.

¥J 1 Diagram 'fJZ diagram

Claims (1)

[Claims] 1. A monochromator that has a slit that divides the X-ray beam generated from the X-ray source into two directions, and that reflects each of the X-ray beams that are divided into the two directions by the slit, and the monochromator that reflects the X-ray beam. each X
Limiting the X-ray irradiation area in a single crystal lattice constant measurement device in which the ray beam is arranged so that the diffraction conditions can be satisfied by multiple single crystals fixed on the same rotating table. The slit is a horizontally wide rectangular slit,
1. A lattice constant measuring device characterized in that a slit insertion mechanism having a structure in which the movement direction is parallel to the lateral direction is disposed.