JPH0731140B2 - Energy-dispersive X-ray diffractometer - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial field of application) The present invention measures the texture of a sample such as a metallic material at any location on the surface of the sample, the reverse pole figure and its distribution chart, or the positive pole figure. The present invention relates to an energy dispersive X-ray diffractometer used for this purpose.

(Prior Art) An X-ray diffractometer for measuring the texture of a metal material is one in which a sample stage to which a sample is attached is continuously rotated around a normal axis of the sample stage by using one motor. There is one in which three motors are used to rotate about the normal axis of the sample stage and about the horizontal axis, and further, it is possible to vibrate in a specific direction within the plate surface of the sample.

These sample stands are used by being attached to an X-ray goniometer. The goniometer is provided with a solar slit that limits the vertical divergence of the incident X-ray beam and a divergence slit that limits the lateral divergence of the incident X-ray beam. The sample area on the sample becomes rectangular. However, the irradiation area can be circularly expanded by rotating the sample.
Generally, the diameter of the irradiation circle is as large as around 10 mm.
Diffracted X-rays from the sample are detected by an X-ray detector after passing through a scattering slit that controls left and right scattering, a solar slit that restricts upper and lower scattering, and a light receiving slit.
As described above, the rotating sample table is provided with five slits. Therefore, as described above, the average texture of the texture measured and analyzed by the X-ray diffractometer in which the sample table is rotated by one motor is used. The inverse pole figure is generally used as a representation method. Further, when the sample table is operated by using three motors, special slits may be added to the five slits similar to the above case, so that the incident X-ray is irradiated on the sample surface. Area becomes rectangular or parallelogram. In this case, the largest side of the irradiation area is
The positive electrode diagram is generally used as a method of expressing an average texture measured and analyzed by an X-ray diffractometer equipped with a sample stage of this type having a size of about 10 mm.

By the way, texture control in the manufacturing process of metallic materials is an effective means for improving the material quality, and many studies have been conducted as a result, and as a result, the texture in each manufacturing process is uneven in location. Has been revealed to occur in. However, as described above, the X-ray diffractometer equipped with the conventional sample stage can only obtain information on the average texture of the material, and cannot obtain information on the local and desired regions. That is, X having the sample table as described above
In the line diffractometer, it was not possible to measure and analyze the inverse pole figure and its distribution chart, which correspond to the location of the material, and the positive pole figure because the movable range of the sample stand was limited.

In some materials, the texture may be distributed at an angle of several degrees with respect to the plate surface, but the conventional X-ray diffractometer generally measures the texture distributed parallel to the plate surface of the material. Therefore, it was not possible to quickly and quantitatively measure the texture that is inclined with respect to the plate surface.

(Problems to be Solved by the Invention) The present invention solves the problems in the conventional X-ray diffractometer as described above, and a reverse pole figure and a distribution chart and a positive pole figure of a local and desired region on the sample surface. It is designed to be able to perform measurement and analysis such as.

(Means for Solving the Problem) The present invention is an energy dispersive X-ray diffraction system in which a sample mounted on a sample stage is irradiated with an X-ray beam and diffracted X-rays emitted from the sample are received. In the device, the X-ray beam intersects the horizontal axis, the vertical axis, and the three orthogonal axes of the normal axis (origin)
And a moving mechanism for moving the sample table in a horizontal direction and a vertical direction in parallel with the sample table on which a sample surface is arranged on a plane including an intersection (origin) of three orthogonal axes. Having a wiring through a slip ring provided in a cylinder on a normal axis for driving a moving mechanism, and rotating a sample table holding mechanism for holding the sample table about a normal axis and a horizontal axis. And a mechanism for rotating the entire sample stage holding mechanism about a vertical axis. When all rotation angles of the sample table holding mechanism around each of the three orthogonal axes are zero degrees, the horizontal translation of the sample table matches the horizontal axis of the sample table holding mechanism, and the horizontal movement in the vertical direction is the sample. It corresponds to the vertical axis of the table holding mechanism. The present invention will be described in detail below with reference to an embodiment apparatus shown in the drawings. FIG. 1 is an explanatory view showing the configuration of the X-ray diffraction apparatus of the present invention, in which X-rays 6 emitted from the X-ray generator 1 are sampled on a sample table 4 from a pinhole 3 provided at the tip of a thin tube 2. Irradiate. Reference numeral 7 is a diffracted X-ray emitted from the sample, which is detected by the semiconductor detector 9 via the light-receiving slit 8. Further, the detection signal is input to a calculation device 15 through an amplifier 11 and a multi-channel analyzer 12 and is calculated, and the result is displayed on a display device 13 such as an XY plotter. 5 is a goniometer, 10 is a high voltage device, and 14 is an interface. The present invention measures the texture of the material in this way,
The mechanism for moving the sample table is characteristic. FIG. 2 is a perspective view of a sample stage moving mechanism example used in the apparatus of the present invention, FIG. 3 (a) is a front view thereof, and FIG. 3 (b) is a side view. The sample table 4 in the present invention is vertically and horizontally movable, and the holding mechanism for holding the sample table is configured to be rotatable about a vertical axis, a horizontal axis and a normal axis. That is, 16 is a bracket for holding the entire sample stage moving mechanism, which is rotated by the motor 24 about the vertical axis 25. Further, a U-shaped bracket 17 is pivotally supported on the bracket 16, and the bracket 17 can be rotated about a horizontal shaft 30 by a motor 26 attached to the bracket 16. The bracket 17 also has a cylinder 33 on the normal axis.
Further, a gear 35 and a bracket 21 for controlling the vertical movement of the sample table 4 are attached to the cylinder 33. Further, a motor 28 is attached to the bracket 21, and the driving force thereof causes the screw 22 to rotate via the coupling 32, so that the bracket 18 screwed into the screw 22 moves in the vertical direction. The bracket 18 also has a screw that connects to the motor 29 attached to the end of the bracket 18 via a coupling 31.
Since 19 is provided and the sample table 4 is screwed into the screw 19, the sample table 4 is moved laterally by the rotation of the screw 19. Note that 20 and 23 are guides provided in parallel with the screws 19 and 22, respectively. A motor 27 is attached to the bracket 17, and its shaft has a gear fitted to the cylinder 33.
Since the gear 36 which meshes with the gear 35 is attached, the gear 36 is rotated by the rotation of the motor 27, and the gear 35 is rotated, and as a result, the bracket 21 (simultaneously the bracket 18) is rotated. In addition, 34 is a slip ring provided on the cylinder 33, the motor 28 and the motor without the leads 37 and 38 being entangled.
It is for supplying current to 29.

Therefore, an operation of setting the sample table at a predetermined position will be described. First, in order to move the sample table 4 laterally, the motor 29 attached to the bracket 18 is normally or reversely rotated. That is, when the motor 29 is normally or reversely rotated, its rotation is transmitted to the screw 19 via the coupling 31, and as a result, the sample table 4 screwed to the screw 19 is rotated on both sides thereof as the screw 19 rotates. It moves laterally by being guided by a guide 20 provided in parallel with. To move the sample table 4 in the vertical direction, the motor 28 attached to the bracket 21 is rotated. That is, when the motor 28 is rotated, the rotation is transmitted to the screw 22 via the coupling 32, and as a result, the bracket 18 engaged with the screw 22 is guided by the guide 23 provided in parallel with the screw 22. Move vertically. Therefore, by appropriately rotating the motors 28 and 29, the sample table 4
The upper sample can be set accurately at the X-ray irradiation position. Further, in the present invention, when the texture of the sample to be observed is not parallel to the plate surface of the sample table but is inclined, the motor
By appropriately rotating 24, 26, 27 and rotating the brackets 16 and 17, the inclination can be corrected and the measurement can be performed. That is, when the motor 26 attached to the bracket 16 is rotated, the bracket 17 pivotally supported by the horizontal shaft 30 thereof rotates in the front-rear direction about the horizontal shaft 30. When the motor 27 attached to the bracket 17 is rotated, the rotation is transmitted to the cylinder 33 via the gear 36 attached to the shaft and the gear 35 meshing with the gear, and as a result, the bracket 18 attached to the cylinder 33 and 21 will rotate. Also motor
Rotation of 24 causes bracket 16 to pivot left (or right) through its vertical axis 25, resulting in the bracket 16
The bracket 17 that is connected to the bracket 17, the bracket 21 that is connected to the bracket 17, and the bracket 18 that is screwed to the bracket 21 with the screw 22 rotate about the vertical shaft 25 as they are. In this way, by rotating the motors 24, 26, 27 as appropriate, the sample table 4 provided on the bracket 18 can be rotated about any of the three axes of the horizontal axis and the vertical axis normal axis to observe the texture. The angle of the sample table 4 can be changed according to the inclination.

Further, the irradiation area of the incident X-ray 6 on the sample surface in the present invention can be changed by exchanging the pinhole 3. That is, there are pinholes with a diameter of 5 μm to 3 mmφ, which are located immediately before the sample. As another means, the diameter of the pinhole is made constant, the thin tubes 2 and 2'are formed into a telescope shape, and the length is changed by changing the length of the thin tube 2 and 2'to make the incident X.
It is also possible to change the irradiation area of the line. The light-receiving slit 8 corresponds to the size of the incident X-ray beam, and the size of the slit is 5 μm to 3 mmφ or 5
The width is μm to 3 mm.

In this way, the three orthogonal axes of the sample table 4 (horizontal axis, vertical axis,
The texture can be measured by aligning and setting the three orthogonal axes (X, Y, Z) of the sample with respect to the normal axis and then irradiating the origin of the three orthogonal axes with X-rays.

(Effects of the Invention) As described above, according to the energy dispersive X-ray analysis apparatus of the present invention, 5 μmφ to 3 mmφ is placed at an arbitrary position on the sample surface.
It is possible to perform on-line automatic measurement / analysis of the inverse pole figure of the area by irradiating the thin-bundle X-ray beam. At that time, by oscillating the horizontal axis and the vertical axis and rotating around the normal axis, the texture existing at a position inclined several degrees from the sample surface is also detected, and the inverse pole figure thereof is also obtained.

When the inverse pole figure as described above is obtained for the entire surface of the sample or a part thereof, a map of the axial density for each crystal orientation corresponding to the optical texture of the sample surface can be obtained.
That is, with this device, not only the measurement and analysis of the reverse pole figure at an arbitrary place on the sample surface but also the crystal orientation topography can be obtained. Furthermore, based on the information obtained from the crystal orientation topograph obtained in advance, 5 μmφ ~ 3 mm to any place on the same sample surface
It is possible to obtain a plurality of local positive electrode dot diagrams simultaneously by irradiating a φ fine-bundle X-ray beam and performing arbitrary rotations around the irradiation region around three orthogonal axes (horizontal axis, vertical axis, normal axis). The effect is great.

[Brief description of drawings]

1 is an explanatory view of an energy dispersive X-ray diffractometer of the present invention, FIG. 2 is a perspective view of a sample stage moving mechanism used in the present invention, FIG. 3 (a) is a front view of the same, and FIG. FIG. 4 is a side view, and FIG. 4 is an explanatory view showing a relationship between an incident light beam slit and a light receiving slit in the device of the present invention. 1: X-ray generator, 2, 2 ': Capillary tube 3: Pinhole, 4: Sample stage 5: Goniometer, 6: X-ray 7: Diffracted X-ray, 8: Receiving slit 9: Semiconductor detector, 10: High Voltage device 11: Amplifier 12: Multi-channel analyzer 13: Display device, 14: Interface 15: Arithmetic device, 16: Bracket 17: Bracket, 18: Bracket 19: Screw, 20: Guide 21: Bracket, 22: Screw 23: Guide , 24: Motor 25: Vertical axis, 26: Motor 27: Motor, 28: Motor 29: Motor, 30: Horizontal axis 31: Coupling, 32: Coupling 33: Cylindrical, 34: Slip ring 35: Gear, 36: Gear 37: Lead wire, 38: Lead wire

Claims (1)

[Claims] 1. An energy dispersive X-ray diffractometer in which a plate-shaped sample mounted on a sample stage is irradiated with an X-ray beam and diffracted X-rays emitted from the sample are received.
A mechanism that irradiates the intersection point (origin) of the three orthogonal axes of the horizontal axis, the vertical axis, and the normal axis with the X-ray beam, and a sample stand on which the sample surface is placed on a plane including the intersection point (origin) of the three orthogonal axes And a moving mechanism for translating the sample stage in the horizontal and vertical directions is provided, and wiring for driving the moving mechanism is provided via a slip ring provided in a cylinder on the normal axis and holds the sample stage. The present invention is characterized in that a mechanism for rotating the sample stage holding mechanism around a normal axis and a mechanism for rotating the sample stage around a horizontal axis are provided, and further a mechanism for rotating the entire sample stage holding mechanism around a vertical axis is provided. Energy dispersive X-ray diffractometer.