JP3928855B2 - Horizontal goniometer sample holder rotating device and X-ray device - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a sample holder of a horizontal goniometer and a θ-θ scan type X-ray apparatus including the sample holder, and more particularly to a rotation mechanism of the sample holder.
[0002]
[Prior art]
In X-ray diffraction, analysis such as substance identification is performed by irradiating a sample with X-rays and detecting diffracted X-rays obtained from the sample. In this X-ray diffraction, a θ-θ scan type X-ray apparatus is known that detects a diffracted X-ray while scanning an incident angle. This θ-θ scan type X-ray apparatus includes an X-ray source that emits X-rays, and calculates an incident angle of X-rays incident on a sample, an emission angle of X-rays diffracted by the sample, and an X-ray intensity. A horizontal goniometer to measure is provided. The intensity of the diffracted X-ray is measured by a counter, and analysis is performed based on the detection signal.
[0003]
In a horizontal goniometer, a sample is supported horizontally, and an X-ray source and a detector are rotated in opposite directions around an X-ray irradiation point on a vertical plane.
The horizontal goniometer includes a sample holder for holding the sample. This sample holder needs to perform optical axis adjustment to align the vertical position with respect to the optical axis connecting the X-ray source and the detector. Therefore, the sample holder needs to be rotated 180 degrees in a direction orthogonal to the optical axis. Therefore, the conventional sample holder is configured to be directly fixed to the rotation center axis of the horizontal goniometer via a bearing.
[0004]
5 and 6 are a schematic view and a perspective view for explaining the outline of a conventional horizontal goniometer and a θ-θ scan type X-ray apparatus provided with the horizontal goniometer. 5A is a front view of the horizontal goniometer, FIG. 5B is a cross-sectional view of the horizontal goniometer, and FIG. 5C is an enlarged view of a mounting portion of the sample holder. FIG. 6 is a perspective view showing the rotation state of the sample holder portion. Note that FIG. 5C corresponds to a portion surrounded by a circle in FIG.
[0005]
In FIG. 5, the horizontal goniometer has a goniometer rotation center shaft 13 in a horizontal direction with respect to a support portion 12 erected on a base 11, and two arms 14, with the goniometer rotation center shaft 13 as a rotation center, 15 are rotated in opposite directions. An X-ray source 16 and a detector 17 provided at each end of the arms 14 and 15 rotate around an X-ray irradiation point on a vertical plane. Light for aligning the position of the X-ray source and the X-ray slit held by the X-ray source with respect to the rotation center of the sample holder 22 and the center of the goniometer rotation center axis 13 in order to align the X-ray irradiation point with the rotation center. Axis adjustment is performed.
[0006]
The sample holder 22 is directly fixed to the rotation center shaft 13 of the horizontal goniometer via the bearing portion 24. In FIG.5 (c), the sample holder 22 is provided with the support surface 22a which supports a sample (not shown), and the holder board 22b which fixes a sample to the support surface 22a. In the optical axis adjustment, the X-ray source is set so that the detection output of the detector 17 becomes equal when the optical axis adjustment plate (not shown) fixed to the support surface 22a is rotated at 0 degree and 180 degrees. The X-ray slit held by the X-ray source is rotated and adjusted around the X-ray source.
[0007]
The support portion 12 is provided with a bearing portion 24 on an extension of the goniometer rotation center shaft 13, and a sample holder rotating plate 25 is attached to the bearing portion 24. A sample holder 22 is fixed to the sample holder rotating plate 25 by a fixed plate 23. Positioning at 0 degrees and 180 degrees is performed by the pins 18 attached to the sample holder rotating plate 25 coming into contact with the holder rotating positioning plate 26.
[0008]
Therefore, the sample holder 22 is attached to the goniometer rotation center shaft 13 by the bearing portion 24 together with the fixed plate 23 and the sample holder rotation plate 25, and the sample holder rotation plate 25 is rotated during the optical axis adjustment, so that the sample holder 22 and the sample holder 23 are rotated together. The holder 22 is rotated integrally. FIG. 6 shows the rotation state of the sample holder 22, and as indicated by an arrow A in the drawing, the sample holder 22 is a bearing portion (not shown in FIG. 6) together with the fixed plate 23 and the sample holder rotation plate 25. ), And thereby the optical axis is adjusted.
[0009]
[Problems to be solved by the invention]
Since the conventional sample holder rotating mechanism is configured to attach the sample holder 22 to the fixed plate 23 and the sample holder rotating plate 25 and directly fix them to the rotation center shaft 13 of the horizontal goniometer via the bearing portion 24. The bearing portion 24 supports the sample holder 22, the fixed plate 23, and the sample holder rotating plate 25 on one side with respect to the support portion 12, and a large moment is applied to the bearing portion 24.
[0010]
Therefore, the conventional sample holder rotation mechanism cannot obtain sufficient rigidity, the sample holder is displaced as shown by arrow B in FIG. 6, and the analysis position deviates from the rotation center of the horizontal goniometer. There is. In particular, in a configuration in which the sample holder can be replaced, when a heavy sample holder is attached, the positional deviation becomes larger.
[0011]
SUMMARY OF THE INVENTION Accordingly, an object of the present invention is to solve the above-described conventional problems and to prevent a shift of the analysis position from the rotation center in the rotation mechanism of the horizontal goniometer. Another object of the present invention is to increase the rigidity of a mechanism that holds the sample holder in rotation.
[0012]
[Means for Solving the Problems]
According to the present invention, the sample holder itself is rotatably held with respect to the fixed portion, so that the mounting portion of the sample holder has sufficient rigidity, and a bearing for rotation required by the conventional rotation mechanism is provided. It is unnecessary.
[0013]
The sample holder rotating device of the horizontal goniometer of the present invention is a rotating device that rotates the sample holder of the horizontal goniometer at least 180 degrees, and directly holds the rotating portion of the sample holder so as to be rotatable with respect to the fixed portion. The rotating shaft and the rotating shaft of the horizontal goniometer are made independent from each other.
[0014]
The fixed part includes a holder fixing plate and a bearing part. The sample holder is attached to the fixed portion by fitting the rotating portion with the holder fixing plate at the shaft portion so that the rotating portion is rotatable with respect to the bearing portion and the bearing portion is fixed to the holder fixing plate. As a result, the sample holder is rotationally supported.
[0015]
Further, by pressing the rotating portion in the axial direction with the O-ring against the bearing portion, the rotating portion can be rotated with respect to the bearing portion, and the positioning at a predetermined position can be freely held. Prevents shakiness of the rotating part in the axial direction. Positioning of the sample holder at 0 degree and 180 degrees can be performed by contact between the plunger provided on the holding part and the rotating part.
Further, the θ-θ scan type X-ray apparatus of the present invention includes the sample holder rotating device of the horizontal goniometer.
[0016]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.
FIG. 1 is a schematic view for explaining an outline of a sample holder rotating device of a horizontal goniometer of the present invention and a θ-θ scan type X-ray apparatus equipped with the sample holder rotating device. 1A is a front view of the horizontal goniometer, and FIG. 1B is a cross-sectional view of the horizontal goniometer. 2 is an enlarged view of the sample holder rotating device, FIG. 3 is an exploded view of each part of the sample holder rotating device, and FIG. 4 shows the rotation state of the sample holder by the sample holder rotating device. FIG. Note that FIG. 2 corresponds to the circle in FIG.
[0017]
In FIG. 1, a horizontal goniometer 10 has a goniometer rotation center shaft 13 in a horizontal direction with respect to a goniometer support portion 12 erected on a base 11, and has two arms with the goniometer rotation center shaft 13 as a rotation center. 14 and 15 are rotated in opposite directions.
[0018]
An X-ray source 16 and a detector 17 provided at each end of the arms 14 and 15 rotate around an X-ray irradiation point on a vertical plane. In order to align the X-ray irradiation point with the rotation center, optical axis adjustment is performed to align the positions of the X-ray source and the X-ray slit with respect to the rotation center of the sample holder 2 and the center of the goniometer rotation center axis 13.
[0019]
The sample holder 2 is attached to the holder fixing portion 8 fixed to the support portion 12 so that the sample holder 2 can be freely rotated by the sample holder rotating device 1 and can be positioned at a predetermined position.
[0020]
2 and 3, the sample holder 2 includes a support surface 2a that supports a sample (not shown), and a holder plate 2b that fixes the sample to the support surface 2a. In the optical axis adjustment, an X-ray source is used so that the optical axis adjustment plate (not shown) fixed to the support surface 2a has the same detection output from the detector 17 at the 0 ° and 180 ° rotation positions. The X-ray slit held by the X-ray source is rotated and adjusted around the X-ray source.
[0021]
The sample holder rotating device 1 holds the sample holder 2 so as to be rotatable in an angle range of at least 180 degrees on the extension of the goniometer rotation center shaft 13 and to be positioned at angular positions of 0 degrees and 180 degrees. The sample holder rotating device 1 includes a sample holder 2, a rotating part 3, and a bearing part 4, and is rotatably attached to a holder fixing plate 8 fixed to a support part 12 of a horizontal goniometer 10. The sample holder rotating device 1 can be replaced in units according to the size, shape, analysis content, etc. of the sample to be analyzed. The attachment of the bearing portion 4 to the holder fixing plate 8 can be performed by fixing means such as screws as shown in FIG.
[0022]
The sample holder 2 is attached to one end of the rotating unit 3 in the axial direction by a fixing means such as a screw. Further, the other end of the rotating portion 3 in the axial direction is attached to the bearing portion 4 so as to be rotatable. The rotating part 3 is attached to the bearing part 4 by the shaft part 5. The shaft portion 5 includes a shaft 5a and a shaft pin 5b. One end side of the shaft pin 5b is press-fitted and fixed in an opening formed in the axial direction of the shaft center in the rotating portion 3, and the other end side is formed in the axial direction at the shaft center of the shaft 5a. The inserted opening is rotatably inserted.
[0023]
The shaft 5a is inserted into the opening formed in the holder fixing plate 8 and the bearing portion 4 with the shaft center aligned, and is fixed to the bearing portion 4 with screws or the like.
In addition, the axis alignment of the axial center of the opening part formed in the holder fixing | fixed part 8 and the bearing part 4 and the rotating shaft center of a goniometer can be performed by positioning of each structural member of the holder fixing | fixed part 8 and the bearing part 4. FIG. .
[0024]
In order to hold the rotating unit 3 rotatably with respect to the bearing unit 4, the rotating unit 3 is rotatably attached to the bearing unit 4 by the holding unit 9. The holding portion 9 is formed in a ring shape, the opening is passed through the outer peripheral portion of the rotating portion 3, the O-ring 6 is sandwiched between the flange portion at one end of the rotating portion 3, and the bearing portion 4 is fixed by a fixing means such as a screw. Install. The O-ring 6 presses the end surface of the rotating portion 3 against the end surface of the bearing portion 4 by its elastic force, and rotatably supports the rotating portion 3 with respect to the bearing portion 4 about the axis center as a rotation center. Shaking of the portion 3 in the axial direction is prevented.
[0025]
A plunger 7 is attached to the holding portion 9, and a portion (not shown) that contacts the plunger 7 is formed on the inner surface of the rotating portion 3. This abutting portion is provided at an angle of approximately 180 degrees with respect to the axis center, for example, in accordance with the support surface 2a of the sample holder 2. When the rotating part 3 is rotated with respect to the bearing part 4, the plunger 7 comes into contact with the contact part at an angular position of 0 degrees or an angular position of 180 degrees. The sample holder 2 is rotationally positioned by this contact.
[0026]
Therefore, according to the sample holder rotating device of the present invention, the sample holder 2 can be rotated with respect to the holder fixing plate 8 by the shaft 5a and the shaft pin 5b, and can be rotated and positioned at a predetermined angular position. it can. In addition, since it can be rotated and supported independently of the goniometer rotation center shaft 13 of the horizontal goniometer 10, the rigidity of the rotation mechanism can be increased, and even when a heavy sample holder is attached, It is possible to prevent the support surface from deviating from the rotation center of the analysis position.
[0027]
At the time of adjusting the optical axis, an optical axis adjusting plate (not shown) is attached to the support surface 2a, and the rotating portion 3 is rotated with respect to the bearing portion 4 and the holder fixing plate 8. The rotating unit 3 can rotate while being held at a predetermined position by the restoring force of the O-ring 6 pressed with the holding unit 9. Therefore, only the sample holder 2 and the rotating unit 3 rotate, and the holding unit 9, the bearing unit 4, the holder fixing unit 8, and the support unit 12 are maintained in a fixed state.
[0028]
FIG. 4 shows the rotation state of the sample holder 2, and the sample holder 2 is rotatably supported by the bearing portion 4 together with the rotation portion 3. As shown by the arrow C in the figure, the rotation position is such that one of the support surfaces 2a of the sample holder 2 faces downward (FIG. 4 (a)) and the other faces upward (FIG. 4 (b)). Optical axis adjustment is performed.
[0029]
According to the sample holder rotating device of the present invention, it is possible to reduce the bearing mechanism by eliminating the need for a bearing portion provided with a bearing or the like for rotating the sample holder, thereby increasing the rotation accuracy and reducing the number of parts.
[0030]
In addition, according to the sample holder rotating device of the present invention, the rotating part to which the sample holder is attached is configured to rotatably support the fixed part, whereby the weight of the apparatus itself can be reduced and the sample can be reduced. The rigidity of the holding portion that holds the holder rotating device can be increased, the bending moment due to the weight of the rotating device can be reduced, and the displacement of the sample holder portion can be reduced.
[0031]
In the above embodiment, the support portion is erected with respect to the base. However, as long as the support unit is independent of the rotation center axis of the horizontal goniometer, the support portion is not limited to erection and can be provided in the lateral direction.
[0032]
【The invention's effect】
As described above, according to the present invention, in the rotation mechanism of the horizontal goniometer, the rigidity of the holding portion of the sample holder can be increased, and the shift of the analysis position from the rotation center can be prevented.
[Brief description of the drawings]
FIG. 1 is a schematic diagram for explaining an outline of a sample holder rotating device of a horizontal goniometer of the present invention and a θ-θ scan type X-ray apparatus equipped with the sample holder rotating device.
FIG. 2 is an enlarged view of a sample holder rotating device of the present invention.
FIG. 3 is an exploded view of each part of the sample holder rotating device of the present invention.
FIG. 4 is a view showing a rotation state of a sample holder by the sample holder rotating device of the present invention.
FIG. 5 is a schematic diagram for explaining an outline of a conventional horizontal goniometer and a θ-θ scan type X-ray apparatus including the horizontal goniometer.
FIG. 6 is a perspective view for explaining a conventional rotation mechanism of a sample holder.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 ... Sample holder rotation apparatus, 2 ... Sample holder, 2a ... Support surface, 2b ... Holder plate, 3 ... Rotation part, 4 ... Bearing part, 5 ... Shaft part, 5a ... Shaft pin, 5b ... Shaft, 6 ... O-ring , 7 ... Plunger, 8 ... Holder fixing plate, 10 ... Horizontal goniometer, 11 ... Base, 12 ... Supporting part, 13 ... Goniometer rotation center axis, 14 ..., 15 ... Arm, 16 ... Tube, 17 ... Detector, 18 DESCRIPTION OF SYMBOLS ... Pin, 22 ... Sample holder, 22a ... Support surface, 22b ... Holder plate, 23 ... Fixed part, 24 ... Bearing part, 15 ... Sample holder rotating plate, 26 ... Holder rotation positioning plate

Claims (4)

A rotating device for rotating a sample holder of a horizontal goniometer at least 180 degrees,
A sample holder rotating apparatus for a horizontal goniometer, wherein the rotating portion of the sample holder is directly held rotatably with respect to a fixed portion, and the rotating shaft of the sample holder and the rotating shaft of the horizontal goniometer are independent from each other. The fixed part includes a holder fixing plate and a bearing part,
The rotating part is rotatable with respect to the bearing part;
The sample holder rotating device for a horizontal goniometer according to claim 1, wherein the bearing portion is fixed to a holder fixing plate.   The sample holder rotating device for a horizontal goniometer according to claim 2, wherein the rotating portion presses the bearing portion in the axial direction by an O-ring. A θ-θ scan type X-ray apparatus comprising the horizontal goniometer sample holder rotating device according to claim 1.

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