JPH0114533B2 - - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION By making a parallel X-ray beam incident on a minute portion on the surface of a polycrystalline sample and detecting the diffracted X-rays, the minute portion can be analyzed and the point of incidence of the X-rays can be When moving, we can know the distribution of matter. In such a diffraction, since the incident area of the X-ray is small, the number of crystal grains involved in the diffraction is extremely small, which tends to cause large errors in measurement. The present invention significantly increases the number of crystal grains involved in diffraction by rotating or rocking the sample in at least two directions while keeping the incident point and angle of X-rays on the sample surface constant. Therefore, it is an object of the present invention to provide an apparatus which can eliminate the above-mentioned drawbacks and which can also easily measure the texture of crystals or the strain of microscopic parts.

Figure 1 is a front view of an embodiment of the present invention, Figures 2 and 3 are
The figures are A-A and B-B cross-sectional views in FIG. It is connected to 5. The worm 3 is screwed onto a support 6 that is attached to move along the rail 4, an X-ray detector 7 is attached to the support, and a slit 8 is formed in the front of the detector.
is provided. In addition, there is an X-ray collimator 9 on the pillar 1.
is attached parallel to the guide rail 4, and a cylindrical shaft 10 is attached to the column 2 on the axis of the collimator. This collimator 9 and cylindrical shaft 10
The belt 15 is rotatably supported at both ends of the arc-shaped guide rail 11, and the pulley 12 attached to one end is connected to the pulley 14 attached to the shaft of the motor 13.
It is connected with. A holding stand 16 is slidably attached to the above-mentioned guide rail 11, a screw 17 is provided for fixing this at an arbitrary position, and a motor 18 is mounted on the holding stand. The sample 20 is attached to a sample stand 19 fixed to the shaft of this motor 18, and a mechanism (not shown) is provided to adjust the position by slightly moving the sample 20 in any direction on the sample stand. be. Further, the arc-shaped guide rail 1
1 is formed so as to have its center on the axis of the collimator 9.

In the above-described apparatus, when setting the sample 20, the holding table 16 is moved on the guide rail 11, so that the rotation axis a of the sample table 19 is aligned with the axis b of the collimator 9, so that the thin parallel line formed by this collimator is aligned. An X-ray detector 21 is set at a position perpendicular to the X-ray beam at a point p, and behind the cylindrical shaft 10. In this state, X-rays are irradiated through the collimator 9 in the direction of arrow x, and the position of the sample 20 is adjusted by observing the output of the detector 21 so that its surface is on the axis b. Further, the X-ray detector 7 is replaced with an optical microscope, and the worm 3 is rotated to move it to a position opposite to the point p. In this state, the surface of the sample is observed using the microscope, and the sample is moved so that the position to be analyzed coincides with the point p.

Next, for X-ray diffraction measurement, the X-ray detector 7
At the same time, the holding table 16 is moved on the guide rail 11 so that the X-ray beam passing through the collimator 9 is incident on the surface of the sample 20 at a desired angle. In this state, by driving the worm 3 intermittently, for example, the detector 7 is fed in steps parallel to the axis b along the guide rail 4, and the output pulses of the detector are counted every time the detector 7 is stopped. At the same time, the pulleys 14 and 12 rotate continuously at a relatively high speed on the sample stage 19 about the axis a.
The guide rail 11 is driven by a motor 13 via a belt 15, and is rotated back and forth, for example, within a range of 150 degrees about the axis b. Through such an operation, the relationship between the intensity of the X-ray x' diffracted on the surface of the sample 20 and detected by the detector 7 and the position of the detector is measured. Further, by moving the sample 20 on the sample stage 19 and repeating the above-mentioned measurement, it is possible to know the distribution state of the substance on the sample surface. Note that the rotation of the sample stage 19 is stopped and the holding stage 1 is
6 on the guide rail, the incident angle of the X-rays x incident on the sample surface changes. Therefore, by observing minute changes in the diffraction angle of the same diffraction line before and after that, the internal strain of the minute portion on the sample surface can be measured. Furthermore, the orientation of the crystal can be determined by fixing the holding table 16 and the detecting part 7 at a suitable fixed position and rotating the guide rail 11 or the sample table 19 little by little around the axis b or a. .

FIG. 4 is a diagram illustrating the operation of the apparatus as described above, in which when the holding table 16 is moved on the guide rail 11, the incidence of a thin parallel X-ray beam x that is incident on a point p on the surface of the sample 20 is The angle θ changes. If the diffracted X-ray x' is detected by the detector 7 while keeping this incident angle constant, the crystal lattice plane that contributes to the diffraction is the 2nd line of the X-rays x and x' as represented by the group of parallel lines q. It is perpendicular to the equisector c. When the sample stage 19 is rotated around the axis a, this axis a will move to a point p on the sample surface.
Since the rotation is perpendicular to the surface of the sample, the bisector c draws a circle d and rotates as shown by the arrow. Therefore, all crystals having lattice planes perpendicular to the rotating bisector c contribute to the diffraction. Furthermore, since the X-rays x are irradiated along the axis b, the guide rail 1 is
1, the bisector c draws an arc e centered on the axis b and rotates as shown by the arrow.
A crystal having a lattice plane perpendicular to the bisector at each position contributes to diffraction.

In this way, the device of the present invention provides at least the above-mentioned a.
The sample is rotated or reciprocated around the two axes b, and the number of crystals contributing to diffraction increases significantly. Therefore, errors can be prevented when measuring the diffraction x-ray intensity of a minute portion, and accurate observation can be performed. Furthermore, as described above, it is possible to easily measure the material distribution on the sample surface, or observe internal strain, crystal orientation, etc. In addition, since the X-ray detector is directly moved, the apparatus can be constructed simply and compactly.

[Brief explanation of drawings]

Figure 1 is a front view of an embodiment of the present invention, Figures 2 and 3 are
The figures are A-A and B-B in Fig. 1, respectively.
The cross-sectional view and FIG. 4 are diagrams illustrating the operation of the present invention. In the figure, 3 is a worm, 4 is a guide rail, 5 is a pulse motor, 7 is an X-ray detector, 9
1 is a collimator, 11 is a guide rail, 13 is a motor, 18 is a motor, 19 is a sample stage, and 20 is a sample.

Claims (1)

[Claims] 1 A collimator that forms a thin parallel X-ray beam and makes the beam incident on the sample surface, a sample stage on which the sample is attached, and an X-ray detector are moved linearly to detect the X-rays diffracted by the sample. means for determining the position of the specimen; means for rotating the specimen stage about a straight line passing through the X-ray incident point on the specimen surface and perpendicular to the specimen surface; and rotating the specimen stage back and forth around the X-ray beam. and means for setting a desired diffraction angle position by rotating the sample stage about a straight line on the sample surface that passes through the X-ray incident point and is perpendicular to the X-ray beam. Microscopic X-ray diffraction device for polycrystalline samples.