JP2010117368A - X-ray diffraction apparatus and x-ray adjusting method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an X-ray diffraction apparatus with a smaller amount of movement required for X-ray adjustment and with a smaller amount of time required for X-ray adjustment. <P>SOLUTION: The X-ray diffraction apparatus including a horizontal goniometer to carry out θ-θ scanning is configured to include a rolling mechanism 5 that rotates an X-ray source 2 on an axis of rotation orthogonal to a direction in which the X-ray source 2 emits X rays, wherein X-ray adjustment is carried out through the rotation of the X-ray source 2 by the rolling mechanism 5. The rolling mechanism 5 changes the direction of X-ray radiation by rotating the X-ray source 2. By changing the direction of X-ray radiation through rotational movements, the amount of movement required for X-ray adjustment and the amount of adjusting time required for X-ray adjustment are reduced. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

The present invention relates to an X-ray diffractometer, and more particularly to adjustment of a goniometer.

In an X-ray diffractometer, X-rays emitted from an X-ray source are irradiated to an analysis position of a sample, and X-rays diffracted at the analysis position are detected by a detector. A mechanism such as a horizontal goniometer is used as a mechanism for equalizing the incident angles of the X-ray source and the detector with respect to the analysis position. Usually, such an X-ray diffractometer that scans a sample with a horizontal goniometer is called a θ-θ scan type X-ray device, and the sample is fixed on the goniometer central axis of the horizontal goniometer on the sample mounting portion. The goniometer is adjusted so that the X-rays irradiated from the X-ray source pass through the analysis position on the sample.

Conventionally, X-ray adjustment by a goniometer is performed by moving the X-ray source itself up and down so that incident X-rays pass through the sample analysis position. Therefore, the goniometer provided in the conventional X-ray diffractometer is provided with a vertical mechanism that moves the X-ray source in the vertical direction.

In the conventional X-ray diffractometer, the X-ray adjustment is performed so that the X-ray from the X-ray source is irradiated to the analysis position of the sample by moving the X-ray source in the vertical direction by the vertical mechanism. Since the vertical mechanism performs position adjustment by moving X-rays in parallel, there is a problem that a large amount of movement is required in the vertical direction and that the adjustment time becomes long.

Accordingly, the present invention aims to solve the above-described conventional problems, and to reduce the amount of operation required for X-ray adjustment in an X-ray diffraction apparatus, and to reduce the adjustment time required for X-ray adjustment. Objective.

The present invention includes a rotation mechanism that rotates an X-ray source , and changes the X-ray irradiation direction by rotating the X-ray source and a slit through which X-rays emitted from the X-ray source are rotated by the rotation mechanism. To do. By changing the irradiation direction of X-rays by a rotation operation, the operation amount required for X-ray adjustment and the adjustment time required for X-ray adjustment are reduced. X-ray diffraction apparatus of the present invention provides an X-ray diffraction apparatus for performing theta-theta scan includes a horizontal goniometer, an X-ray source and a direction perpendicular to the X-ray emission direction of the X-ray source as a rotation axis direction and the X-ray source And a rotation mechanism that rotates a slit through which X-rays emitted from the X-ray are rotated, and X-ray adjustment is performed by rotation of the X-ray source by the rotation mechanism and a slit through which X-rays emitted from the X-ray source pass. .

The rotation mechanism changes the X-ray emission direction by rotating the X-ray source and the slit through which the X-rays emitted from the X-ray source pass , thereby changing the X-ray irradiation position with respect to the analysis position of the sample. adjust. The X-ray source is rotated with the direction orthogonal to the X-ray emission direction of the X-ray source as the rotation axis direction. The amount of X-ray movement at the X-ray irradiation position is determined by the product of the rotation angle of the X-ray source and the distance between the X-ray source and the irradiation position. In the vertical movement by the conventional vertical mechanism, it is necessary to move by almost the same amount as the adjustment amount, whereas in the X-ray diffraction apparatus of the present invention, the X-ray source and the X-ray emitted from the X-ray source are transmitted. The X-ray position can be adjusted by slightly adjusting the rotation angle of the slit to be passed. One form of the rotation mechanism can be configured by rotating the X-ray source around the rotation axis with an adjustment screw. For example, a micrometer can be used as the adjustment screw, and fine adjustment is also possible.

In the X-ray adjustment method of the X-ray diffractometer according to the present invention, a jig for shielding a part of the X-ray is disposed at the analysis position, and the jig is orthogonal to the incident X-ray at the analysis position and the horizontal Two rotational positions differing by 180 degrees around the rotational axis in the same direction as the goniometer central axis of the goniometer, and the X-ray dose passing through the jig is measured at each rotational position. When the X-ray source, the sample analysis position, and the detector are aligned on a straight line, the measured X-ray doses at two rotation positions different by 180 degrees of the jig are equal. Therefore, the X-ray source is rotated with the direction orthogonal to the X-ray emission direction as the rotation axis direction, and the rotational position of the X-ray source is adjusted so that the X-ray measurement amounts at the rotational positions of the two jigs have a predetermined relationship.

According to the aspect of the present invention, it is possible to perform adjustment with a small amount of operation and to shorten the adjustment time as compared with the conventional vertical mechanism. Further, the rotation mechanism according to the present invention can reduce the number of parts as compared with the conventional vertical mechanism, so that the rotation mechanism can be reduced in weight, and the burden on the drive unit that drives the goniometer can be reduced.

As described above, according to the X-ray diffraction apparatus of the present invention, the amount of operation required for X-ray adjustment can be reduced, and the adjustment time required for X-ray adjustment can be reduced.

It is the schematic for demonstrating the X-ray-diffraction apparatus of this invention. It is a figure for demonstrating the operation | movement by the rotation mechanism of this invention, and the jig | tool used for X-ray adjustment using a rotation mechanism. It is a figure for demonstrating the operation | movement by the rotation mechanism of this invention, and the jig | tool used for X-ray adjustment using a rotation mechanism. It is a flowchart for demonstrating the X-ray adjustment method of the X-ray-diffraction apparatus by this 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 X-ray diffraction apparatus of the present invention, and shows a position where a horizontal goniometer is viewed backward. The X-ray diffractometer 1 includes an X-ray source 2 that irradiates a sample S placed on a sample stage (not shown) with X-rays, and a detector 3 that detects diffracted X-rays diffracted by the sample S. Are configured to be attached to the horizontal goniometer 4, and the present invention includes a rotation mechanism 5 that rotates the X-ray source 2.

The rotation mechanism 5 is a mechanism that rotates the X-ray source 2 and the slit 2a through which the X-rays emitted from the X-ray source 2 are narrowed and passed around the rotation axis R, around the rotation axis provided in the goniometer 4. It can be set as the structure supported so that rotation is possible, and it can be rotationally driven by arbitrary drive means. As the driving means of the rotation mechanism 5, for example, a position deviated from the rotation axis R is pushed or pulled by an adjustment screw 6 such as a micrometer, and the rotation amount is determined according to the amount of movement of the adjustment screw 6, or It can be set as the structure which rotates the rotating shaft R directly or via a gearwheel.

The rotation axis R of the rotation mechanism 5 is a direction perpendicular to the X-ray emission direction of the X-ray A emitted from the X-ray source 2, and is provided on the X-ray emission axis on the X-ray source 2, for example. . Note that the rotation axis R is not necessarily arranged on the X-ray source 2 or the X-ray emission axis, and is arranged at a position away from the X-ray source 2 or at a position away from the X-ray emission axis. It can also be configured. When the rotating mechanism 5 is rotated, the irradiation direction of the X-ray A emitted from the X-ray source 2 is changed, and the irradiation position P of the X-ray on the sample S can be adjusted.

Next, the operation | movement by the rotation mechanism of this invention and the jig | tool used for the X-ray adjustment using a rotation mechanism are demonstrated using FIG. 2, FIG. In the X-ray adjustment method of the X-ray diffractometer of the present invention, the rotation amount of the rotation mechanism is adjusted using the half jig 7. The half jig 7 is configured by providing a rotating support 7d with a shield 7a. By rotating the rotating support 7d 180 degrees, the first surface 7b is set to the upper position or the second surface 7c is set to the upper position. Can be positioned as The half jig 7 is attached to the sample analysis position, and is arranged between the X-ray source 2 and the detector 3. A part of the X-ray A emitted from the X-ray source 2 is shielded by the shield 7a of the halving jig 7, but a part of the X-ray is detected by the detector 3 without being shielded by the shield 7a. Is done.

Here, when the height of the surface of the first surface 7b is set to the height of the analysis position of the sample, the X-ray dose that passes through the shield 7a depends on the analysis position, and the incident X-rays are incident on the analysis position. You can know the state.

2 (a), 2 (b) and 3 (a), 3 (b) show the case where the direction of the emission X-ray from the X-ray source with respect to the analysis position is aligned, and FIG. 3C and 3D show a case where the direction of the emission X-ray from the X-ray source with respect to the analysis position is not aligned. When the direction of the emitted X-ray is correctly set with respect to the analysis position, as shown in FIGS. 2 (a) and 3 (a), the rotary support 7d of the half jig 7 is rotated, When the first surface 7b is positioned so as to face upward, the detector 3 detects X-rays passing upward from the analysis position with the analysis position as a boundary. The detected X-ray dose is an amount proportional to the width indicated by d1 in FIG.

On the other hand, as shown in FIGS. 2B and 3B, when the rotation support 7d of the half jig 7 is further rotated 180 degrees and positioned so that the first surface 7b faces downward, the detector 3 detects X-rays passing downward from the analysis position with the analysis position as a boundary. The detected X-ray dose is an amount proportional to the width indicated by d2 in FIG. If the direction of the emitted X-ray is correctly set with respect to the analysis position, the two detected X-ray doses (a quantity proportional to d1 and a quantity proportional to d2) are equal. Therefore, when the X-ray dose detected in FIG. 3A and FIG. 3B detected by changing the rotational position of the half jig 7 is equal, the direction of the emitted X-ray of the X-ray source is It can be determined that the analysis position is set correctly.

On the other hand, when the direction of the emitted X-ray of the X-ray source is not correctly set with respect to the analysis position, as shown in FIGS. 2 (c) and 3 (c), the first surface 7b is When the detector 3 is positioned so as to face upward, the detector 3 detects X-rays passing upward from the analysis position with the analysis position as a boundary. At this time, since the direction of the emitted X-ray of the X-ray source is deviated, the detected X-ray dose becomes an amount proportional to the width indicated by d3 in FIG.

On the other hand, as shown in FIG. 3 (d), when the rotary support 7d of the half jig 7 is rotated 180 degrees and positioned so that the first surface 7b faces downward, the detector 3 is located at the analysis position. X-rays passing below from the analysis position are detected. At this time, since the direction of the emitted X-ray of the X-ray source is deviated, the detected X-ray dose is an amount proportional to the width indicated by d4 in FIG. If the direction of the emitted X-ray is not set correctly with respect to the analysis position, there is a difference between the two detected X-ray doses (a quantity proportional to d3 and a quantity proportional to d4).

Therefore, when the X-ray dose (amount proportional to d3 and a proportion proportional to d4) detected in FIG. 3 (c) and FIG. 3 (d) detected by varying the rotation position of the half jig 7 is different. Therefore, it can be determined that the direction of the emitted X-ray of the X-ray source is not set correctly with respect to the analysis position.

FIGS. 2D, 3E, and 3F show the case where the direction of the emission X-ray from the X-ray source with respect to the analysis position is aligned according to the present invention. As shown in FIGS. 2 (c), 3 (c) and 3 (d) above, when the direction of the emitted X-ray of the X-ray source is not set correctly with respect to the analysis position, the rotation mechanism of the present invention is By rotating the radiation source, the direction of the emitted X-ray of the X-ray source is correctly set with respect to the analysis position.

When the direction of the emission X-ray is not set correctly with respect to the analysis position, the rotation mechanism 5 is rotated as shown in FIGS. 2D, 3E, and 3F to release the X-ray emission direction. To change. This rotation changes the incident angle of the emitted X-ray with respect to the half jig 7. This is detected when the rotary support 7d of the half jig 7 is positioned so that the first surface 7b faces upward, and the detector 3 detects X-rays passing upward from the analysis position with the analysis position as a boundary. The X-ray dose changes from an amount proportional to the width indicated by d3 in FIG. 3C to an amount proportional to the width indicated by d5 in FIG.

On the other hand, as shown in FIG. 3 (f), when the rotation support 7d of the half jig 7 is positioned so that the first surface 7b faces downward, the detector 3 moves downward from the analysis position with the analysis position as a boundary. When the passing X-ray is detected, the detected X-ray dose is changed from an amount proportional to the width indicated by d4 in FIG. 3D to an amount proportional to the width indicated by d6 in FIG. Change.

Next, an X-ray adjustment method of the X-ray diffraction apparatus according to the present invention will be described with reference to the flowchart of FIG. In the X-ray adjustment method of the X-ray diffraction apparatus according to the present invention, first, in a state where the sample is not attached, the half jig 7 is attached to the analysis position of the sample (Step S1), and the rotary support 7d is placed on the surface (first surface). 7b (or the first surface 7c) is positioned and set to face upward (step S2), then X-rays are emitted from the X-ray source 2 and passed through the shield 7a of the halving jig 7. The line is detected by the detector 3, and the count number n1 is measured (step S3).

Next, the rotary support 7d is rotated 180 degrees and positioned and set so that the back surface (the first surface 7c (or the first surface 7b)) faces upward (step S4). The detector 3 detects the X-rays that have been emitted and passed through the shield 7a of the half jig 7, and the count number n2 is measured (step S5). When the measured count numbers n1 and n2 are compared and it is determined that there is a difference between n1 and n2 (step S6), the X-ray source is rotated by the rotation mechanism (step S7), and the above-described steps S2 to S2 are performed. Repeat S6.

When the measured count numbers n1 and n2 are compared and it is determined that n1 and n2 are equal, the alignment of the direction of the emission X-ray with respect to the analysis position is completed (step S6). After the alignment of the direction of the emitted X-ray with respect to the analysis position is completed, the incident angle of the X-ray with respect to the sample is set by the goniometer in steps S8 to S10. FIG. 3 (g) shows this angle setting.

After removing the halving jig used in each step (step S8), the goniometer is adjusted to adjust the incident angle θs to the X-ray sample (step S9), and the detection intensity is measured by the detector (step S9). S10) Steps S9 and S10 are repeated so that the detected intensity becomes a peak value (step S11). When the detected intensity reaches a peak value, the incident angle θs with respect to the X-ray sample is set to an optimum angle. At this time, the incident angle θd with respect to the detector is set to the same angle as θs by the function of the goniometer.

DESCRIPTION OF SYMBOLS 1 ... X-ray-diffraction apparatus, 2 ... X-ray source, 2a ... Slit, 3 ... Detector, 4 ... Horizontal goniometer, 5 ... Rotation mechanism, 6 ... Adjustment screw, 7 ... Half jig, 7a ... Shielding part, 7b ... 1st surface, 7c ... 2nd surface, A ... X-ray, P ... Analysis position, R ... Rotating shaft, S ... Sample.

Claims (2)

In an X-ray diffractometer that includes a horizontal goniometer and performs a θ-θ scan ,
The X-ray diffractometer includes an X-ray source and a slit through which X-rays emitted from the X-ray source pass.
The emission X at two rotational positions which are arranged at the sample analysis position, orthogonal to the emission X-rays emitted by the X-ray source, and different by 180 degrees around the rotation axis in the same direction as the goniometer central axis of the horizontal goniometer A half jig that shields part of the wire;
A mechanism for adjusting the position of the X-ray source and the slit so that the X-ray dose detected by the detector at the two different rotational positions of the half jig has a predetermined relationship;
The mechanism for adjusting the position can rotate the X-ray source and the slit at a position different from the goniometer central axis of the horizontal goniometer, with the direction orthogonal to the X-ray emission direction of the X-ray source as the rotation axis direction. A rotating mechanism that supports
An X-ray diffraction apparatus for performing X-ray adjustment for adjusting an irradiation position of X-rays passing through the slit by rotation of the X-ray source and the slit by the rotating mechanism. Place a jig to shield part of the X-rays at the analysis position,
The jig shields at least a part of the incident X-rays at two rotation positions that are orthogonal to the incident X-ray and are 180 degrees around the rotation axis in the same direction as the goniometer central axis of the horizontal goniometer. Measure the X-rays that pass through
The X-ray source and the X-ray emitted from the X-ray source are passed through the measurement, with the direction orthogonal to the X-ray emission direction of the X-ray source at a position different from the goniometer central axis of the horizontal goniometer. Rotate the slit and perform
X-ray adjustment is performed to adjust the irradiation position of the X-ray passing through the slit by adjusting the rotation position of the X-ray source so that the X-ray measurement amount at the two rotation positions of the jig has a predetermined relationship. An X-ray adjustment method for an X-ray diffractometer characterized by the above.

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