JP3553362B2 - X-ray analyzer - Google Patents

Description

[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to an X-ray analyzer for obtaining a pole figure.
[0002]
[Prior art]
Each crystal grain of the polycrystalline aggregate usually has an orientation different 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.
[0003]
The center part of the pole figure shown in FIG. 1 is obtained by the reflection method (Schulz method) by Schulz, and its peripheral part is obtained by the transmission method (Decker-Asp-Haker method) by Decker, Asp, and Harker.
[Problems to be solved by the invention]
The reflection method is an optical system using a divergent X-ray beam, while the transmission method is an optical system using a parallel X-ray beam. 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 a slit exchange operation is a very troublesome operation for the operator.
[0004]
The present invention has been made in view of such a point, and an object of the present invention is to provide an X-ray analyzer capable of continuously obtaining a pole figure by an unmanned person.
[0005]
[Means for Solving the Problems]
An X-ray analyzer according to the present invention for achieving this object includes an X-ray source for irradiating a sample with X-rays, an X-ray detector for detecting diffracted X-rays from the sample, the X-ray source and the sample. A first slit interposed therebetween, a second slit interposed between the sample and the X-ray detector, and a slit width control means for controlling a slit width of the first slit and the second slit. And a third slit; third slit control means for disposing the third slit between the first slit and the sample and retracting the third slit from the position; a sample table on which the sample is mounted; An X-ray analyzer comprising: sample control means for controlling the position of the sample stage for analyzing a sample by a transmission method; and pole figure creating means for creating a pole figure of the sample based on the output of the X-ray detector. An apparatus, wherein the slit width control means is configured to The slit width of the first slit and the second slit is controlled according to the analysis method, and the third slit control means controls the third slit to the first slit when the sample is analyzed by the reflection method. When the sample is analyzed by a transmission method while being disposed between the slit and the sample, the third slit is retracted from that position.
[0006]
BEST MODE FOR CARRYING OUT THE INVENTION
Hereinafter, embodiments of the present invention will be described with reference to the drawings.
[0007]
2 and 3 are views for explaining the X-ray analyzer of the present invention. FIG. 2 shows a case where a sample is analyzed by a reflection method, and FIG. 3 shows a case where a sample is analyzed by a transmission method. It is a figure showing the case. Each of the configurations shown in FIGS. 2 and 3 is arranged 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 a second slit 5 is provided between the X-ray detector 4 for detecting diffracted X-rays from the sample and the sample 2. Are located. 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, and the sample stage 7 is placed on a turntable 8 rotatable about an axis B passing through the center of the sample stage 7 and perpendicular to the sample surface. I have. The rotation of the turntable 8 is performed by a turntable rotating means 9.
[0009]
The turntable 8 is placed on a tilt stage 10, and the tilt stage 10 is attached to the 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, and the rotation of the rotary stage 11 is performed by a rotary stage rotating unit 13. Note that the rotary stage 11 is attached to the base 6.
[0010]
Reference numeral 14 denotes a third slit which is a length limiting slit. The third slit 14 is attached to the rotating stage 11, and the third slit 14 is disposed between the first slit 3 and the sample 2 during analysis by a reflection method.
[0011]
Reference numeral 15 denotes a slit width control unit. The slit width control unit 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, which creates an extreme figure as shown in FIG. 1 based on the output of the X-ray detector 4.
[0012]
As described above, the configuration of the apparatus shown in FIGS. 2 and 3 has been described. The configuration 7 to 12 constitute a sample control unit, and the rotary stage 11 and the rotary stage rotating unit 13 form a third slit control unit. Be composed. 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 controlled by a central control device (CPU), not shown.
[0013]
Next, the operation of the device having such a configuration will be described.
[0014]
First, a case where a sample is analyzed by a reflection method will be described with reference to FIG.
[0015]
As shown in FIG. 2, the optical system based on the reflection method is an equal-angle reflection optical system in which the incident angle and the diffraction angle are each θ with 2θ as the diffraction angle. 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.
[0016]
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.
[0017]
When the adjustment of the slit width is completed, the sample is irradiated with X-rays. Then, when the B axis is defined as α = 90 ° when the B axis is on a plane determined by the incident X-rays and the diffracted X-rays, the inclination means 12 adjusts the angle from 90 ° to 30 °, for example. The tilt stage 10 is rotated clockwise by 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.
[0018]
As described above, each crystal grain on the sample is oriented in various directions, and the α rotation about the A axis in the sample plane and the β rotation about the B axis normal to the sample plane as described above. When the crystal grain comes to a position that satisfies the diffraction condition at the time of the operation, the X-ray diffraction from the crystal grain is detected by the X-ray detector 4. In some samples, each crystal grain is oriented in a specific direction. In such a case, many diffracted X-rays are detected at a certain position. The pole figure creating means 16 gives a numerical value proportional to the pole density to a position corresponding to the pole figure based on the output of the X-ray detector 4.
[0019]
As described above, 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 °. This is for blocking diffracted X-rays. The measurement at the remaining angles of 0 ° to 30 ° is performed by the transmission method described below.
[0020]
Next, the sample analysis by the transmission method will be described with reference to FIG.
[0021]
When analyzing a sample by the transmission method, the rotating stage rotating means 13 rotates the rotating stage 11 90 ° clockwise from the state of FIG. Due to the rotation of the rotary stage 11, the third slit 14 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.
[0022]
By the rotation of the rotating stage 11 described above, the optical system becomes an optical system based on a transmission method as shown in FIG. 3, and the optical system based on the transmission method irradiates the sample 2 with X-rays passing through the first slit 3, An X-ray detector 4 detects the diffracted X-ray that has passed through the sample and passed through the second slit 5.
In such an optical system, the slit width control means 15 adjusts the slit width d1 so that the first slit 3 becomes a parallel X-ray width slit. Further, the slit width control means 15 adjusts the second slit width d2 to an optimum slit width.
[0023]
When the adjustment of the slit width is completed, the sample is irradiated with X-rays. When the sample position at which the incident X-ray and the diffracted X-ray are symmetric with respect to the sample surface is defined as α = 90 °, the tilting stage 10 tilts the tilt stage 10 so that α changes from 30 ° to 0 °. Are rotated by 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.
[0024]
When the α rotation about the A axis in the sample plane and the β rotation about the B axis of the normal to the sample plane are performed, when the crystal grain comes to a position satisfying the diffraction condition, Diffracted X-rays from the crystal grains are detected by the X-ray detector 4. The pole figure creating means 16 gives a numerical value proportional to the pole density to a position corresponding to that of the pole figure based on the output of the X-ray detector 4. The results of the analysis by the transmission method and the analysis by the transmission method are represented as pole figures as shown in FIG.
[0025]
As described above, the X-ray analyzer of the present invention has been described with reference to FIGS. 2 and 3. In such an X-ray analyzer, the slit width of the first and second slits is automatically set according to the analysis method. In addition, since the third slit is automatically retracted during the transmission method, a pole figure can be obtained continuously without an operator.
[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 ... Rotary table, 9 ... Rotary 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)

An X-ray source for irradiating the 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, A second slit disposed between the X-ray detectors, a slit width control means for controlling a slit width of the first slit and the second slit, a third slit, and the third slit. A third slit control unit disposed between the first slit and the sample and retracted from the position, a sample table on which the sample is mounted, and a sample table for analyzing the sample by a reflection method and a transmission method. An X-ray analysis apparatus comprising: sample control means for controlling a position; 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: The first slit and the second slit according to the analysis method. The slit control means controls the slit width of the slit, and the third slit control means arranges the third slit between the first slit and the sample while analyzing the sample by the reflection method, while transmitting the sample. An X-ray analyzer characterized by retracting the third slit from its position when performing analysis by a method. 2. The X-ray according to claim 1, wherein when the sample is analyzed by switching from the reflection method to the transmission method, the sample control means rotates the sample stage by 90 degrees around an axis perpendicular to the sample surface. Analysis equipment.

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