JP2002131250A - X-ray diffraction equipment - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an X-ray diffraction equipment fit for large samples, in which large samples can be moved in a small space and a stress in a direction normal to the direction of X-ray beams can be measured for large samples. SOLUTION: The X-ray diffraction equipment 1 which has a horizontal goniometer 4 and carries out θ-θ scanning, include an R-θ stage 9 for moving at least a sample mounting part 5 linearly in a horizontal direction and moving to rotate the part 5 about a perpendicular axis, and a rotary moving stage 10 for supporting the R-θ stage 9 and rotating the stage 9, so that the stage can be positioned at two angular positions separated by 90 deg. about the normal axis passing through an analysis position.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an X-ray diffractometer, and more particularly to a stage suitable for a large sample.

[0002]

2. Description of the Related Art In an X-ray diffractometer, an X-ray emitted from an X-ray source is irradiated to an analysis position of a sample, and the X-ray diffracted at the analysis position is detected by a detector. X for this analysis position
A mechanism such as a horizontal goniometer for performing a θ-θ scan for equalizing the respective incident angles of the radiation source and the detector is used. Normally, the center position of this θ-θ scan is the analysis position. In this horizontal goniometer, the analysis position where X-rays are irradiated is fixed, and it is necessary to move the sample in a two-dimensional direction in order to align an analysis point on the sample with the analysis position. Conventionally, the movement of the sample is performed by a stage that moves in the x and y directions.

On the other hand, stress measurement is known as an application example using an X-ray diffraction apparatus. When an internal stress is present in a material, the crystal plane spacing of the crystals constituting the material changes.
When the X-ray diffraction line obtained by irradiating this material with X-rays is measured, the material moves from the reflection position in a state where there is no stress, and its width increases. In the X-ray stress measurement, the stress is measured from the change in the X-ray diffraction line. The change in the lattice spacing is obtained from the diffraction angle that satisfies the Bragg condition, and the strain and stress can be obtained by calculation. . The diffraction angle and intensity distribution of the X-ray diffraction line can be obtained by a goniometer.

Conventionally, when measuring stress in an X-ray diffractometer, measurement is performed in two directions, that is, the direction of the X-ray beam and the direction perpendicular to the X-ray beam, by using the swinging side method. The side tilting method makes it possible to measure the bottom of a gear, an uneven portion, and the like, which are difficult to measure by the parallel tilting method, by making a plane determined by a sample surface normal and a stress measurement direction orthogonal to a scanning surface of a detector. (For example, see JP-A-6-13
No. 7966) Further, by measuring the sample while swinging it, the number of crystal grains contributing to diffraction can be increased, and the diffraction intensity can be increased.

[0005]

The conventional X-ray diffractometer has a problem in handling a large sample in the sample movement and stress measurement. When moving a large sample in a conventional X-ray diffraction apparatus, the moving stage on which the large sample is placed moves in the x direction and the y direction. It is necessary to make the rectangle as large as the size of the sample, and there is a problem that the space required only for movement becomes large and the apparatus becomes large.

In the case of measuring the stress of a large sample in a conventional X-ray diffractometer, when the sample is swung in a direction perpendicular to the X-ray beam direction, the center of rotation (center of rotation) depends on the weight of the sample itself. There is a problem of deviation, and when measuring in two directions, the direction of the X-ray beam and the direction perpendicular to the X-ray beam, there is a problem that the direction perpendicular to the X-ray beam direction cannot be determined. For example, when analyzing a crack or a pressed state from stress measurement, the stress measurement direction is defined as the direction perpendicular to the measurement crack or the radial direction of the press, and if the stress measurement direction shifts, accurate stress measurement Becomes difficult.

Accordingly, an object of the present invention is to solve the above-mentioned conventional problems and to provide an X-ray diffraction apparatus suitable for a large sample. In particular, an object of the present invention is to provide an X-ray diffractometer capable of moving a large sample in a small space, and to perform a stress measurement of a large sample in a direction perpendicular to the X-ray beam direction. It is intended to provide a device.

[0008]

SUMMARY OF THE INVENTION The present invention provides an X-ray diffraction apparatus equipped with a horizontal goniometer for performing a .theta .-. Theta. Scan, which enables a two-dimensional movement with a small amount of movement and / or a rotational movement about an analysis position. An X-ray diffraction apparatus suitable for a large sample is provided by providing a sample moving stage to be used. In the θ-θ scan by the horizontal goniometer, the incident angles of the X-ray source and the detector with respect to the analysis position are made equal to θ, and scanning is performed on a plane including the X-ray beam by changing the θ.

According to a first aspect of the present invention, there is provided an X-ray diffractometer having a horizontal goniometer for performing a θ-θ scan, wherein at least a sample mounting portion is moved linearly in a horizontal direction and rotated around a vertical axis. It is configured to include a θ stage. The R-θ stage can be configured to include an R-direction drive unit and a θ-direction drive unit. The R-θ stage performs horizontal linear movement by the R-direction drive unit, and rotates by a θ-direction drive unit about a vertical axis. I do. The linear movement in the horizontal direction and the rotation movement around the vertical axis can be performed independently of each other. A configuration in which the R-direction drive unit is provided on the θ-direction drive unit, or the θ-direction drive is mounted on the R-direction drive unit Any of the configurations in which the unit is provided can be adopted.

By combining two movements, a linear movement in the horizontal direction and a rotational movement about the vertical axis, the movement between the two points is replaced by an arc movement instead of the conventional orthogonal (x, y) linear movement. This can reduce the area of the space required only for movement. Therefore, according to this aspect, a large sample can be moved in a small space.

A second aspect of the present invention is configured to include a rotary movement stage that rotates so as to be positionable at two angular positions forming 90 degrees about a vertical axis passing through the analysis position. The rotary moving stage may be configured to include a fixed portion and a rotating portion rotatably supported on the fixed portion so as to be rotatable around a vertical axis passing through the analysis position. The rotating part can be positioned at two positions at an angle of 90 degrees with respect to the fixed part.

When stress is measured on a sample in two directions of an X-ray beam direction and a direction perpendicular to the X-ray beam direction, the stress measurement in the X-ray beam direction is performed at one angular position of the rotary moving stage. The stress measurement in the direction perpendicular to the X-ray beam direction is performed by measuring the stress in the X-ray beam direction at the other angular position rotated by 90 degrees on the rotary moving stage. Stress measurement in the X-ray beam direction at the other angular position corresponds to stress measurement in a direction perpendicular to the X-ray beam direction at the angular position before rotation. In this way, the 90
By performing the stress measurement in the X-ray beam direction at the respective angular positions, the stress measurement in the X-ray beam direction and the stress measurement in the direction perpendicular to the X-ray beam direction can be performed. Therefore, according to this aspect, it is possible to perform stress measurement in a direction perpendicular to the X-ray beam direction.

[0013] A third aspect of the present invention comprises a first aspect and a second aspect.
An X-ray diffractometer equipped with a horizontal goniometer and performing θ-θ scanning, wherein an R-θ stage that moves at least a sample mounting portion in a horizontal linear direction and rotates around a vertical axis. And the R-θ
A rotary translation stage is provided for supporting the stage and for rotating around a vertical axis passing through the analysis position so as to be positioned at two angular positions forming 90 degrees. According to this aspect, a large sample can be moved in a small space,
Further, stress measurement in a direction perpendicular to the X-ray beam direction can be performed.

[0014]

Embodiments of the present invention will be described below in detail with reference to the drawings. 1 and 2 show X of the present invention.
FIG. 1 is a schematic diagram for explaining a line diffraction apparatus, and FIG.
Shows a position where the horizontal goniometer is viewed backward, and FIG. 2 shows a position where the horizontal goniometer is viewed sideways. FIG. 1B schematically shows a sample mounting portion and a rotary stage when the X-ray diffraction apparatus shown in FIG. 1A is viewed from above. The X-ray diffraction apparatus 1 includes an X-ray source 2 for irradiating a sample S arranged on a sample mounting portion 5 with X-rays, and a detector 3 for detecting a diffracted X-ray diffracted by the sample S, using a horizontal goniometer. The sample mounting unit 5, which is mounted on the support unit 4 and supported on the support unit 7, includes a rotary moving stage 10 and an R-θ stage 9 provided on a base unit 12.
It is a configuration supported by

The horizontal goniometer 4 is a mechanism for adjusting the angles of the incident X-rays and the outgoing X-rays to the sample S at the same angle, and is fixed to the base 12. The rotary moving stage 10 includes a fixed base 10b and a rotary base 10a rotatable by a bearing 10c with respect to the fixed base 10b.
And the turntable 10a has a vertical axis 14 passing through the analysis position 13.
Is supported rotatably about the rotation axis.

The rotary stage 10 moves the turntable 10a relative to the base 12 and the horizontal goniometer 4 to each other.
Two positioning mechanisms 11 for positioning at an angle of 0 degree
Is provided. The positioning mechanism 11 includes a positioning pin 11a provided on the turntable 10a side, a contact pin 11a fixed on the base portion 12, a leaf spring 11c, and a fixing member 11d for fixing the leaf spring 11c to the base portion 12 side. . 2
The contact pin 11a of one of the positioning mechanisms 11 determines the rotational position of the turntable 10a by contacting the positioning pin 11a, and is located at an angular position of 90 degrees with respect to the vertical axis 14 and rotates. It is installed at a position where it comes into contact with 11a. The leaf spring 11c is a member that holds the positioning pin 11a in contact with the contact pin 11a at a corresponding contact position. Positioning by the positioning mechanism 11 is performed by rotating the turntable 10 a and positioning pins 11.
a is pushed by a force equal to or greater than the elastic force of the spring 11c so that the positioning pin 11a can get over the spring 11c,
This is performed by contacting the contact pin 11a. After the contact, the positioning pin 11a contacts the spring 11c and the contact pin 1
1a, and is held by the elastic force of the spring 11c.

On the other hand, in order to move the positioning pin 11a from the positioning position to the other positioning position, the turntable 1
0a is rotated in the opposite direction with a force greater than the elastic force of the spring 11c, and the positioning pin 11a is moved over the spring 11c. The R-θ stage 9 is arranged above the rotary movement stage 10. R-θ stage 9
Is mounted by fixing the base 8 on the turntable 10a.

The R-θ stage 9 is a stage movable in a linear direction (R direction) and a rotating direction (θ direction), and adjusts the distance to the horizontal goniometer 4 by moving in the linear direction (R direction). Further, by moving in the rotation direction (θ direction), the rotation position with respect to the horizontal goniometer 4 is adjusted. By adjusting the linear direction and the rotation direction, the position of the sample mounting portion 5 supported upward is adjusted in the linear direction and the rotation direction.
The analysis position in the planar direction of the sample S placed on the top is adjusted.

An example of the configuration of the R-θ stage 9 includes an R-direction drive unit 9a and a θ-direction drive unit 9b, an R-direction drive unit 9a is provided on the base 8, and a θ-direction drive unit 9b is further provided.
Note that the arrangement order of the R-direction drive unit 9a and the θ-direction drive unit 9b can be reversed. The R direction drive unit 9a
Drive shaft 9d and drive motor 9 arranged in a linear movement direction
c, and drives the drive shaft 9d by rotating the drive motor 9c to cause the base 12 and the horizontal goniometer 4 to perform linear movement. Further, the θ-direction driving unit 9
Reference numeral b denotes a drive motor 9e, which rotatably supports the reference portion 6 supporting the sample mounting portion 5 on the R-direction drive portion 9a.
By rotating the drive motor 9e, the reference unit 6 is rotated, and the base unit 12 and the horizontal goniometer 4 are rotated.

FIG. 1B shows the moving positions of the rotary moving stage 10 and the sample mounting section 5. The moving position of the sample mounting part 5 is determined by the moving state of the R-θ stage 9,
3 shows a moving state of the rotary moving stage 10. The sample mounting section 5a is located at a position separated from the horizontal goniometer 4 by the R-θ stage 9, and the sample mounting section 5b is a R direction driving section 9 of the R-θ stage 9.
The symbol a indicates a state where the sample is moved from the position of the sample mounting portion 5a to the horizontal goniometer 4 side.

The sample mounting section 5c is provided with the rotary stage 1.
0 indicates a state where the sample is rotated by 90 degrees from the position of the sample mounting portion 5a.
8 shows a state where the sample is moved from the position of the sample mounting portion 5c to the analysis position 13 by the R-direction driving portion 9a. Further, the sample mounting section 5c is rotated at the position of the sample mounting section 5b by the θ-direction drive section 9b of the R-θ stage 9 and then moved parallel to the horizontal goniometer 4 by the R-direction drive section 9a. Can also be moved.

The linear movement of the R-θ stage 9 by the R-direction drive 9a and the θ-direction drive 9b of the R-θ stage 9
Does not have the space for performing only the movement caused by the movement in the x-direction and the movement in the y-direction as in the related art, so that the space in the X-ray diffraction apparatus can be used efficiently. A base 6 is mounted on the θ-direction drive unit 9b of the R-θ stage 9, and a sample mounting unit 5 supported by a support unit 7 is provided on the base 6. The support part 7
It can be composed of columns 7a, 7b, 7c of a predetermined length. By changing the length of the columns 7a, 7b, 7c, the sample can be set at the height of the analysis position 13 in accordance with the thickness of the sample S. The height of the surface can be adjusted.

Next, the operation of the R-θ stage and the operation of the rotary moving stage will be described with reference to FIGS. FIG. 3A shows a stage position corresponding to the sample mounting section 5a in FIG. 1B. Sample mounting part 5a
Is moved away from the horizontal goniometer 4 by the R-direction drive unit 9a of the R-θ stage 9. In addition,
At this time, if the surface of the sample S on the opposite side to the horizontal goniometer 4 direction is denoted by the symbol B and the surface of the sample S when the horizontal goniometer 4 is viewed from the lateral direction is denoted by the symbol A, FIG.
In the state of (a), the side of the symbol A can be seen. FIG.
(B) shows the state of the R-θ stage 9 from the state of FIG.
A state where the directional driving unit 9a has moved to the horizontal goniometer 4 side is shown. The analysis position on the sample S can be adjusted by the movement of the R direction drive unit 9a. In this case, the side of the sample S indicated by the symbol A can be seen.

FIGS. 3C and 3D show the horizontal goniometer 4.
FIG. 3 is a view from the position where the camera is viewed in the lateral direction, and is a state in which the sample is rotated by 90 degrees from the state of FIG. 3A by the rotational movement of the rotary moving stage 10 (the sample mounting portion 5c in FIG. From the state rotated by 90 degrees, further moved parallel to the horizontal goniometer 4 by the R-direction drive unit 9a of the R-θ stage 9 (the sample mounting unit 5d in FIG. 1B).
Is shown. In this case, the side of the sample S with the reference numeral B can be seen.

Next, the positioning operation of the rotary stage will be described with reference to FIG. FIG.
4A and 4C are views of the rotary moving stage viewed from below, and FIGS. 4B and 4D are views of the rotary moving stage viewed from the lateral direction. A positioning pin 11a is attached to a rotary table 10a constituting the rotary moving stage 10 so as to face the fixed table 10b.
The positioning mechanism 11 is provided on the side of the fixed base 10b constituting the “0”. The positioning mechanism 11 includes a contact pin 11b, a leaf spring 11c, and a fixing member 11 for fixing the leaf spring 11c.
d, and are provided opposite to each other at two positions with an angle of 90 degrees therebetween. The contact pin 11b is a member that stops rotation by contacting the positioning pin 11a and positions the rotation position of the turntable 10a at that position, and the contact surface determines the rotation position of the turntable 10a. Therefore, two contact pins 11b
Is positioned and installed so that the position of each surface that contacts the positioning pin 11a is at an angle of 90 degrees.

Further, the leaf spring 11c is attached with its distal end portion slightly spaced from the contact pin 11b, and holds the contacting positioning pin 11a in the gap by elasticity. The elasticity of the leaf spring 11c is set to such a degree that the positioning pin 11a can be moved over by the rotation of the turntable 10a.

FIGS. 4 (a) and 4 (b) and FIGS. 4 (c) and 4 (d)
Indicates a state in which each is at an angle position of 90 degrees. From the rotational positions of FIGS. 4A and 4B, the turntable 10a
Is rotated in the direction of the arrow, the positioning pin 11a overcomes the elasticity of the leaf spring 11c and gets over, thereby being disengaged from one of the positioning mechanisms 11. Turntable 10a
Is rotated by 90 degrees, the positioning pin 11a hits the leaf spring 11c of the other positioning mechanism 11, and the leaf spring 11c
Overcoming the elasticity of the leaf spring 11c to come into contact with the other contact pin 11b.
It is held by the elasticity of By performing the above operation in the reverse direction, it is possible to return to the angular position of FIGS. 4A and 4B again.

Next, the operation of stress measurement by the rotary moving stage will be described with reference to FIG. The stress measurement can be performed in two directions, an X-ray beam direction and a direction perpendicular to the X-ray beam direction. FIGS. 5A and 5B show the sample S
FIG. 5 (a) schematically shows a case where stress measurement is performed in two directions as indicated by thick arrows (a, b) above.
5B and the rotational position in FIG. 5B are in an angular relationship of 90 degrees with each other by the rotary movement stage, and the X-ray beam direction and the scanning surface are shown in the same direction.

At the rotary table position in FIG. 5A, the stress measurement direction a is the X-ray beam direction, and the stress measurement direction b is the direction b perpendicular to the X-ray beam direction. Goniometer is ω
A swing mechanism such as an axis (tilt), a χ axis (rolling), and a φ axis (rotation) is provided. By swinging the sample S by the swing mechanism, the number of crystal grains contributing to diffraction is increased to increase the diffraction intensity. Can be enhanced. When the χ axis is rotated in FIG. 5A, in the case of a large sample, the center of rotation is shifted due to the weight of the sample itself, and the stress measurement direction b cannot be determined.

Therefore, the rotational movement stage of the present invention is rotated by 90 degrees around the analysis position to change the relationship between the stress measurement directions a and b and the X-ray beam direction and the direction perpendicular to the X-ray beam direction. The measurement direction b is the X-ray beam direction, and the stress measurement direction a is a direction perpendicular to the X-ray beam direction. FIG. 5B shows a position state obtained by converting this angular relationship by 90 degrees. According to this position, FIG.
Stress measurement direction b where measurement is difficult at position (a)
In the X-ray beam direction where measurement is possible.

[0031]

As described above, according to the X-ray diffraction apparatus of the present invention, a large sample can be moved in a small space, and a large sample can be moved in a direction perpendicular to the X-ray beam direction. Stress measurement can be performed, and an X-ray diffractometer suitable for a large sample can be obtained.

[Brief description of the drawings]

FIG. 1 is a schematic diagram for explaining an X-ray diffraction apparatus of the present invention.

FIG. 2 is a schematic diagram for explaining the X-ray diffraction device of the present invention.

FIG. 3 is a diagram for explaining an operation of an R-θ stage and an operation of a rotary movement stage by the X-ray diffraction apparatus of the present invention.

FIG. 4 is a diagram illustrating a positioning operation in a rotary movement stage of the X-ray diffraction apparatus according to the present invention.

FIG. 5 is a view for explaining an operation of stress measurement by a rotary movement stage of the X-ray diffraction apparatus of the present invention.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... X-ray diffraction apparatus, 2 ... X-ray source, 3 ... Detector, 4 ... Horizontal goniometer, 5 ... Sample mounting part, 7 ... Support part, 8 ... Base part, 9 ... R-theta stage, 9a ... R direction drive Part, 9b ...
θ-direction drive unit, 9c, 9e: drive motor, 9d: drive shaft, 10: rotary moving stage, 10a: rotary table, 10b
... Fixing base, 10c ... Bearing, 11 ... Positioning mechanism,
11a: positioning pin, 11b: contact pin, 11c ...
Leaf spring, 11d: fixing member, 12: base portion, 13: analysis position, 14: vertical axis.

Claims (3)

[Claims] 1. An X-ray diffractometer having a horizontal goniometer and performing θ-θ scanning, comprising an R-θ stage for moving at least a sample mounting portion in a horizontal linear direction and rotating around a vertical axis. X-ray diffractometer. 2. An X-ray diffractometer having a horizontal goniometer and performing a θ-θ scan, comprising a rotary moving stage that rotates so as to be positioned at two angular positions forming 90 degrees with each other around a vertical axis passing through an analysis position. An X-ray diffraction apparatus, comprising: 3. An X-ray diffractometer equipped with a horizontal goniometer and performing θ-θ scanning, wherein an R-θ stage which moves at least a sample mounting portion in a horizontal linear direction and rotates around a vertical axis; An X-ray diffractometer, comprising: a rotation stage that supports the θ stage and rotates so as to be positioned at two angular positions forming 90 degrees around a vertical axis passing through the analysis position.