JPH11271243A - X-ray analyzer - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an unmanned X-ray analyzer capable of continuously providing a pole point figure. SOLUTION: In analysis by a reflection method, a slit width control means 15 adjusts the slit width d1 so that a first slit 3 may be a divergence X-ray width slit, and also it adjusts the second slit width d2 to the most suitable slit width. In analysis by a transmission method, a rotary stage rotating means 13 rotates a rotary stage 11 clockwise by 90 deg. from the state as shown in the Fig. 2. A third slit 14 is retreated from between the first slit 3 and a sample 2 by the rotation of the rotational stage 11. In the rotation of the rotary stage 11, a rotational table rotating means 9 rotates a rotational table 8 clockwise by 90 deg.. Moreover, the slit width control means 15 adjusts the slit width d1 so that the first slit 3 may be a parallel X-ray width slit, and it adjusts the second slit width d2 to the most suitable slit width.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

TECHNICAL FIELD The present invention relates to an X-ray analyzer for obtaining a pole figure.

[0002]

2. Description of the Related Art Each crystal grain of a polycrystalline aggregate usually has a different orientation from that of its adjacent crystal grains. The orientation of each crystal grain is measured by an X-ray diffractometer, and a pole figure shows the orientation of each crystal grain. FIG. 1 shows an example of the pole figure.

The central part of the pole figure shown in FIG.
It is obtained by a reflection method (Schulz method) using Iz, and its periphery is Decker, Asp, and Harker.
Et al. (Decker-Asp-Haker)
Law).

The reflection method has a divergence X
An optical system using a ray bundle, while the transmission method uses a parallel X
This is an optical system using a ray bundle. Since the optical system is different when these two methods are used in combination, the measurement must be interrupted during the measurement of one pole figure, and the divergent X-ray flux slit must be replaced with a parallel X-ray flux slit. In the analysis by the reflection method, a length limiting slit must be arranged between the divergent X-ray flux slit and the sample. Such slit replacement work is very troublesome for the operator.

The present invention has been made in view of the above points, and an object of the present invention is to provide an X-ray analyzer capable of obtaining an unmanned and continuous pole figure continuously.

[0005]

An X-ray analyzer according to the present invention that achieves this object is an X-ray analyzer for irradiating a sample with X-rays.
A source, an X-ray detector for detecting diffracted X-rays from the sample, a first slit disposed between the X-ray source and the sample, and a first slit disposed between the sample and the X-ray detector. A second slit, slit width control means for controlling a slit width of the first slit and the second slit, a third slit, and the third slit arranged between the first slit and the sample; And third slit control means for retreating from the position, a sample table on which the sample is placed, sample control means for controlling the position of the sample table for analyzing the sample by a reflection method and a transmission method, and An X-ray analysis apparatus comprising: a pole figure creating unit that creates a pole figure of a sample based on an output of an X-ray detector, wherein the slit width control unit is configured to control the first figure according to a method of analyzing the sample. Controlling the slit width of the slit and the second slit, The third slit control means arranges the third slit between the first slit and the sample when the sample is analyzed by the reflection method, and the third slit when the sample is analyzed by the transmission method. The slit is retracted from the position.

[0006]

Embodiments of the present invention will be described below with reference to the drawings.

FIGS. 2 and 3 are views for explaining the X-ray analyzer of the present invention. FIG. 2 shows a case in which a sample is analyzed by a reflection method, and FIG. FIG. 6 is a diagram showing a case where analysis is performed by using FIG. Each of the configurations shown in FIGS. 2 and 3 is disposed in a sample chamber of the X-ray analyzer. 2 and 3, reference numeral 1 denotes an X-ray source attached to a sample chamber wall, and reference numeral 2 denotes a sample. A first slit 3 is arranged between the X-ray source 1 and the sample 2, and an X-ray detector 4 for detecting diffracted X-rays from the sample and the sample 2
A second slit 5 is arranged between them. The X-ray detector 4 is mounted on the wall of the sample chamber. Although not shown, the first slit 3 and the second slit 5 are mounted on a base 6.

[0008] The sample 2 is placed on a sample stage 7,
The sample table 7 is placed on a rotary table 8 that can rotate about an axis B passing through the center of the sample table 7 and perpendicular to the sample surface. The rotation of the turntable 8 is performed by a turntable rotating means 9.

The turntable 8 is placed on a tilt stage 10, and the tilt stage 10 is attached to a rotary stage 11 so as to be tiltable about a tilt axis A. The tilt of the tilt stage 10 is performed by tilt means 12.
The rotary stage 11 is rotatable about the Z axis.
3 is performed. The rotation stage 11 is attached to the base 6.

Reference numeral 14 denotes a third slit which is a length limiting slit. The third slit 14 is attached to the rotary stage 11, and the third slit 14
Is arranged between the first slit 3 and the sample 2 at the time of analysis by the reflection method.

Reference numeral 15 denotes a slit width control means. The slit width control means 15 controls a slit width d1 of the first slit 3 and a slit width d2 of the second slit 5. Reference numeral 16 denotes an extreme figure creating means. The extreme figure creating means 16 creates an extreme figure as shown in FIG. 1 based on the output of the X-ray detector 4.

The configuration of the apparatus shown in FIGS. 2 and 3 has been described above. A sample control means is constituted by the constitutions 7 to 12, and a third slit is constituted by the rotating stage 11 and the rotating stage rotating means 13. Control means is configured. Although not shown, the turntable rotating means 9, the tilting means 12, the rotating stage rotating means 13 and the slit width control means 15 are respectively provided with a central control device (CP
U).

Next, the operation of the device having such a configuration will be described.

First, a case where a sample is analyzed by a reflection method will be described with reference to FIG.

As shown in FIG. 2, in the optical system using the reflection method, the incident angle and the diffraction angle are each set to θ, where 2θ is the diffraction angle.
This is an optical system of equiangular reflection. The optical system based on the reflection method irradiates the sample 2 with X-rays passing through the first slit 3 and the third slit 14, and converts the diffracted X-rays passing through the second slit 5 into an X-ray detector 4. Is an optical system to detect.

In such an optical system, the slit width control means 15 adjusts the slit width d1 so that the first slit 3 becomes a divergent X-ray width slit. Further, the slit width control means 15 adjusts the second slit width d2 to an optimum slit width.

When the adjustment of the slit width is completed,
The sample is irradiated with X-rays. And the inclining means 12
Is defined as α = 90 ° when the B axis is on a plane determined by the incident X-ray and the diffracted X-ray, and the tilt stage 10 is rotated clockwise so that α becomes 90 ° to, for example, 30 °. At a predetermined angle. At this time, the turntable rotating means 9 rotates the turntable 8 by 360 ° every time the tilt stage 10 is rotated by a predetermined angle.

As described above, each crystal grain on the sample is oriented in various directions. Such an α rotation around the A axis in the sample plane and the B axis along the normal line of the sample plane are centered. When the crystal grain comes to a position satisfying the diffraction condition when the β rotation is performed, the X-ray diffracted from the crystal grain is detected by the X-ray detector 4. In some samples, each crystal grain is oriented in a specific direction.
Many diffracted X-rays are detected at a certain position. The pole figure creating means 16 is based on the output of the X-ray detector 4,
A numerical value proportional to the pole density is given to the position corresponding to the pole figure.

Although the sample analysis by the reflection method has been described with reference to FIG. 2, as described above, the rotation of the tilt stage 10 is limited to α = 30 °. Is to block diffraction X-rays. The measurement at the remaining angles of 0 ° to 30 ° is performed by the transmission method described below.

Next, the sample analysis by the transmission method will be described with reference to FIG.

When a sample is analyzed by the transmission method, the rotating stage rotating means 13 rotates the rotating stage 11 90 ° clockwise from the state shown in FIG. Due to the rotation of the rotary stage 11, the third slit 14
It is retracted from between the first slit 3 and the sample 2. When the rotary stage 11 rotates, the turntable rotating means 9 rotates the turntable 8 clockwise by 90 °. Due to the rotation of the turntable 8, the sample position of β = 0 ° in the reflection method becomes the same as β = 0 ° in the transmission method.

By the rotation of the rotary stage 11 described above,
The optical system is an optical system based on a transmission method as shown in FIG.
The optical system based on this transmission method irradiates the sample 2 with X-rays passing through the first slit 3, and detects the diffracted X-rays passing through the sample and passing through the second slit 5 with the X-ray detector 4. It is an optical system. In such an optical system, the slit width control means 15 adjusts the slit width d1 such that the first slit 3 becomes a parallel X-ray width slit. Also,
The slit width control means 15 calculates the second slit width d2
Is adjusted to the optimum slit width.

When the adjustment of the slit width is completed,
The sample is irradiated with X-rays. And the inclining means 12
Defines the sample position at which the incident X-ray and the diffracted X-ray are symmetric with respect to the sample plane as α = 90 °, and rotates the tilt stage 10 by a predetermined angle so that α changes from 30 ° to 0 °. . At this time, the turntable rotating means 9 rotates the turntable 8 by 360 ° every time the tilt stage 10 is rotated by a predetermined angle.

The α around the A-axis in the sample plane as described above
When the crystal grains come to a position that satisfies the diffraction conditions when the rotation and the β rotation about the normal B axis of the sample surface are performed, the diffracted X-rays from the crystal grains are output from the X-ray detector 4. Is detected. The pole figure creating means 16 gives a numerical value proportional to the density of the pole to the position corresponding to the pole figure based on the output of the X-ray detector 4.
Numeral 6 shows the results of the analysis by the reflection method and the analysis by the transmission method as pole figure as shown in FIG.

The X-ray analyzer of the present invention has been described above with reference to FIGS. 2 and 3. In such an X-ray analyzer, the width of the first and second slits depends on the analysis method. Automatically controlled, and the third slit is automatically retracted during the transmission method, so that a pole figure can be obtained continuously and unmanned.

[Brief description of the drawings]

FIG. 1 is a diagram showing an example of a pole figure.

FIG. 2 is a view for explaining an X-ray analyzer of the present invention, and is a view for explaining sample analysis by a reflection method.

FIG. 3 is a view for explaining an X-ray analyzer of the present invention, and is a view for explaining sample analysis by a transmission method.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... X-ray source, 2 ... sample, 3 ... 1st slit, 4 ... X-ray detector, 5 ... 2nd slit, 6 ... Base, 7 ... Sample stage, 8 ... Rotating table, 9 ... Rotating table rotation Means, 10: tilt stage, 11: rotary stage, 12: tilt means, 13: rotary stage rotating means, 14: third slit, 15: slit width control means, 16: pole figure creating means

Claims (2)

[Claims] An X-ray source for irradiating a sample with X-rays,
An X-ray detector for detecting diffracted X-rays from the sample, a first slit disposed between the X-ray source and the sample, and a second slit disposed between the sample and the X-ray detector A slit width control means for controlling a slit width of the first slit and the second slit; a third slit;
Third slit control means for disposing the slit between the first slit and the sample and retreating from the position thereof, a sample table on which the sample is mounted, and analyzing the sample by a reflection method and a transmission method. An X-ray analysis apparatus comprising: sample control means for controlling a position of a sample stage; and a pole figure creating means for creating a pole figure of a sample based on an output of the X-ray detector, wherein the slit width control means comprises: Controlling the slit width of the first slit and the second slit in accordance with the sample analysis method, wherein the third slit control means controls the third slit when the sample is analyzed by the reflection method. An X-ray analyzer, wherein the third slit is retracted from its position when the sample is analyzed by a transmission method while being disposed between the first slit and the sample. 2. The method according to claim 1, wherein when the sample is switched from the reflection method to the transmission method for analysis, the sample control means rotates the sample stage by 90 degrees around an axis perpendicular to the sample surface. 2. The X-ray analyzer according to 1.