JPWO2016152654A1 - X-ray diffraction measurement apparatus and X-ray diffraction measurement method - Google Patents

Abstract

Provided are an X-ray diffraction measurement apparatus and an X-ray diffraction measurement method capable of performing X-ray diffraction measurement on a sample in a desired shape and improving the measurement accuracy. The X-ray diffractometer 1 rotates a sample 10 in a predetermined plane by rotating around a predetermined first rotation axis C1, and X irradiates the rotating sample 10 with X-rays. Diffraction that detects the diffracted X-rays 12 transmitted through the sample 10 and diffracted by moving on the arc trajectory f centered on the source 3 and the second rotation axis C2 orthogonal to the optical axis C0 of the X-ray. In a virtual plane including the X-ray detection unit 4, the optical axis C0, and the second rotation axis C2, the first rotation axis C1 is relatively relative to the optical axis C0 at a predetermined acute angle θ with the sample 10 as the center. And an axis tilt mechanism 5 for tilting.

Description

  The present invention relates to an X-ray diffraction measurement apparatus and an X-ray diffraction measurement method.

  As an analysis method for analyzing the crystal structure, foreign matter, and defects of a sample, X-ray diffraction measurement is known in which a polycrystalline sample is irradiated with X-rays and scattered (diffraction) X-rays from the sample are observed. Yes. In such X-ray diffraction measurement, a glass capillary rotating with a sample enclosed is irradiated with X-rays from a direction orthogonal to the rotation axis, and X-rays transmitted through the sample and diffracted are diffracted X-rays. A measurement method for observing with a detection unit, a measurement method for irradiating a sample rotating on a rotating table with X-rays, and observing X-rays reflected and diffracted from the sample with a diffraction X-ray detection unit, etc. (For example, refer to Patent Document 1).

JP 2003-279506 A

The measurement method for rotating the glass capillary irradiates X-rays from a direction orthogonal to the rotation axis of the glass capillary, so that the observation area of the sample by the diffraction X-ray detector is large. As a result, the number of particles that diffract incident X-rays (particles satisfying the diffraction condition) in the sample increases, so that X-ray diffraction measurement can be performed with high accuracy.
However, in this measurement method, since a glass capillary having a diameter of about 1.0 mm or less is used, it is necessary to finely grind the sample in order to enclose the sample in the glass capillary. For this reason, for example, when it is desired to measure a plate-like sample or the like as it is without being finely ground, it cannot be measured by this measurement method.

On the other hand, the measurement method of rotating the sample on the above-described rotating table does not require fine crushing of the sample, so that even a plate-like sample or the like can perform X-ray diffraction measurement with its shape. However, in this measurement method, X-rays are irradiated onto a sample that rotates on a predetermined plane by a turntable, so the observation area of the sample by the diffraction X-ray detector is small, and the number of particles that satisfy the diffraction condition can be determined by using a glass capillary. Compared to the rotating measurement method. For this reason, in the measuring method rotated on a turntable, there exists a problem that the measurement precision of X-ray diffraction measurement falls.
The present invention has been made in view of the above problems, and an X-ray diffraction measurement apparatus and an X-ray that can perform X-ray diffraction measurement on a sample in a desired shape and can improve the measurement accuracy. The object is to provide a diffraction measurement method.

  The X-ray diffraction measurement apparatus of the present invention rotates around a predetermined first rotation axis, thereby rotating a sample within a predetermined plane, and an X-ray with respect to the sample rotated by the sample rotating unit. The X-ray source that irradiates the sample and the diffraction that detects the diffracted X-rays transmitted through the sample and diffracted by moving on an arc locus centering on a second rotation axis orthogonal to the optical axis of the X-ray In a virtual plane including the X-ray detection unit, the optical axis, and the second rotation axis, the first rotation axis is set to a predetermined acute angle with respect to the optical axis with the sample rotated by the sample rotation unit as a center. And a shaft tilting mechanism that relatively tilts at a degree.

  In the X-ray diffraction measurement method of the present invention, the sample rotating unit rotates around a predetermined first rotation axis so that the sample rotates in a predetermined plane, and the X-ray source rotates the sample. The irradiation step of irradiating the sample rotated by the unit with X-rays, and the diffracted X-ray detection unit moving on an arc locus centering on a second rotation axis orthogonal to the optical axis of the X-ray The sample rotated by the sample rotating section in a virtual plane including a detection step of detecting diffracted X-rays transmitted through the sample and diffracted, and an axis tilt mechanism including the optical axis and the second rotation axis And an axis tilting step of tilting the first rotation axis relative to the optical axis at a predetermined acute angle.

  According to the X-ray diffraction measurement apparatus and the X-ray diffraction measurement method of the present invention, when a sample is irradiated with X-rays, the sample is rotated within a predetermined plane by the sample rotating unit, so that the conventional rotating table is rotated. The sample can be rotated by a method similar to the method. For this reason, unlike the conventional measurement method of rotating a glass capillary, it is not necessary to finely crush the sample, so that the sample can be subjected to X-ray diffraction measurement in a desired shape.

  In addition, the first rotation axis of the sample rotation unit is centered on the sample rotated by the sample rotation unit in the virtual plane including the optical axis of the X-ray and the second rotation axis of the diffraction X-ray detection unit by the axis tilt mechanism. The optical axis can be relatively inclined at a predetermined acute angle. Thereby, compared with the case where the 1st axis of rotation is not inclined to the optical axis, the observation area of the sample by the diffraction X-ray detection part can be expanded. As a result, the number of particles satisfying the diffraction condition can be increased, so that the measurement accuracy of the X-ray diffraction measurement can be improved.

The shaft tilt mechanism is preferably capable of adjusting the acute angle.
In this case, the inclination angle (acute angle) of the first rotation axis with respect to the optical axis can be appropriately adjusted according to the sample.

The acute angle is preferably set in an angle range of 15 to 20 °.
In this case, the observation region of the sample by the diffraction X-ray detection unit can be expanded as much as possible while suppressing the amount of X-ray absorption by the sample.

The sample is preferably in the form of a tablet.
In this case, when measuring a sample having a large amount of X-ray absorption, the amount of X-ray absorption can be adjusted by making the sample into a tablet shape formed by mixing a diluent. . As a result, it is possible to perform accurate X-ray diffraction measurement in which the X-ray absorption amount is corrected.

  According to the present invention, X-ray diffraction measurement can be performed on a sample in a desired shape, and the measurement accuracy can be improved.

It is a schematic block diagram which shows the X-ray-diffraction measuring apparatus which concerns on one Embodiment of this invention. It is a front view which shows a sample rotation apparatus. It is AA arrow sectional drawing of FIG. 3 is a flowchart showing an X-ray diffraction measurement method. It is explanatory drawing which shows the observation area | region of the sample by a diffraction X-ray detection part. It is a graph which shows the experimental result of verification experiment.

Hereinafter, embodiments of the present invention will be described with reference to the drawings.
<X-ray diffraction measurement device>
FIG. 1 is a schematic configuration diagram showing an X-ray diffraction measurement apparatus according to an embodiment of the present invention. In FIG. 1, an X-ray diffraction measurement apparatus 1 includes a sample rotating device 2 that holds a sample 10 rotatably, and an X-ray source 3 that irradiates the sample 10 held by the sample rotating device 2 with X-rays. A diffraction X-ray detector 4 that detects diffracted X-rays transmitted through the sample 10 and an axis inclination that inclines the first rotation axis C1 of the sample rotating device 2 relative to the optical axis C0 of the X-ray. And a mechanism 5.

FIG. 2 is a front view showing the sample rotating device 2. 3 is a cross-sectional view taken along arrow AA in FIG.
2 and 3, the sample rotating device 2 includes a main body portion 21, a sample rotating portion 22 that can rotate with respect to the main body portion 21, and a rotation driving unit 23 that rotationally drives the sample rotating portion 22. doing.

  The main body portion 21 of the present embodiment is formed in a rectangular parallelepiped shape, and has a mounting hole 21c penetrating from the front surface 21a toward the rear surface 21b. The sample rotating portion 22 is rotatably supported around the first rotation axis C1 disposed on the central axis of the mounting hole 21c. A connector 24 to which a power cable or the like of the rotation drive unit 23 is connected is provided on the side surface 21d of the main body unit 21.

The rotation drive unit 23 is composed of, for example, an electric motor, and rotates the sample rotation unit 22 with respect to the main body unit 21 at a high speed in the direction of the arrow in FIG. 2 about the first rotation axis C1. The rotation speed of the sample rotating unit 22 is set to 180 rpm, for example.
The sample rotating portion 22 includes a cylindrical portion 22a that is rotatably supported by a mounting hole 21c of the main body portion 21 via a rolling bearing 25, and an annular plate portion 22b that is detachably attached to the cylindrical portion 22a. Have.

  A hollow portion 22c for allowing X-rays to pass from one axial side (the upper side in FIG. 3) to the other axial side (the lower side in FIG. 3) is formed inside the cylindrical portion 22a. A flange portion 22d is formed at one axial end portion (lower end portion in FIG. 3) of the cylindrical portion 22a. An outer peripheral portion of the annular plate portion 22b is detachably attached to the flange portion 22d by a plurality of (here, four) bolts 26.

  The annular plate portion 22b is a transparent synthetic resin member that can transmit X-rays. The center of the annular plate portion 22b is disposed on the first rotation axis C1 in a state where the annular plate portion 22b is attached to the flange portion 22d. The sample 10 is fixed to the center of the outer surface of the annular plate portion 22b.

  The sample 10 of the present embodiment is made of, for example, a green compact formed by compacting a predetermined amount of fine powder, and the center thereof coincides with the center of the annular plate portion 22b, that is, the first It is fixed to the annular plate portion 22b so as to be disposed on one rotation axis C1. Thus, the sample 10 is rotatably held together with the sample rotating unit 22 in a state of being arranged on the axially outer side (lower side in FIG. 3) of the hollow portion 22c of the cylindrical portion 22a.

  As shown in FIG. 1, the X-ray source 3 is arranged on the rear surface 21 b side of the main body 21 of the sample rotating device 2 with a predetermined distance from the rear surface 21 b in the y-axis direction. The X-ray source 3 has an X-ray optical axis C0 from the rear surface 21b side of the main body 21 along the y-axis direction, the hollow portion 22c of the sample rotating portion 22, the center portion of the annular plate portion 22b, and the sample. It arrange | positions in the position which passes the center part of the sample 10 hold | maintained at the rotation part 22, respectively.

  With the above configuration, the sample 10 is rotated within a predetermined plane (the outer surface of the annular plate 22b) by rotating the sample rotating unit 22 around the first rotation axis C1 with respect to the main body 21 of the sample rotating apparatus 2. be able to. Then, the X-rays emitted from the X-ray source 3 are passed through the hollow part 22c and the annular plate part 22b of the sample rotating part 22 from the rear surface 21b side of the main body part 21 to irradiate the central part of the rotating sample 10 can do.

  In FIG. 1, the diffracted X-ray detection unit 4 is disposed so as to be horizontally movable around a second rotation axis C2 perpendicular to the vertical direction (z-axis direction) with respect to the optical axis C0. Specifically, the diffracted X-ray detector 4 is arranged so as to move on an arc locus f centered on the second rotation axis C2. Thereby, the diffracted X-ray detection unit 4 detects the diffracted X-rays 12 that have been transmitted through the sample 10 and diffracted.

  In FIG. 1, the shaft tilting mechanism 5 is composed of, for example, a goniometer stage. The goniometer stage 5 includes a fixed stage 51 and a movable stage 52 that can move in the y-axis direction with respect to the fixed stage 51. The sample rotating device 2 is placed and fixed on the upper surface of the movable stage 52.

  The movable stage 52 is driven by an actuator (not shown) and moves in an arc in the y-axis direction around the sample 10 held by the sample rotating device 2. Thereby, the first rotation axis C1 of the sample rotating device 2 is a light beam centered on the sample 10 held by the sample rotating device 2 in a virtual plane (yz plane) including the optical axis C0 and the second rotation axis C2. It can be inclined with respect to the axis C0 at a predetermined acute angle θ.

  The goniometer stage 5 can adjust the amount of movement of the movable stage 52 in order to adjust the acute angle θ within an angle range of, for example, 0 to 25 °. However, from the viewpoint of suppressing the amount of X-ray absorption by the sample 10, the acute angle θ is preferably set to an angle range of 15 to 20 °.

<X-ray diffraction measurement method>
FIG. 4 is a flowchart showing an X-ray diffraction measurement method using the X-ray diffraction measurement apparatus 1. Hereinafter, the X-ray diffraction measurement method of the present embodiment will be described with reference to FIG.
First, the sample 10 is attached to the sample rotating unit 22 of the sample rotating device 2 (step S1). Specifically, the sample 10 is attached to the center portion of the annular plate portion 22b of the sample rotating portion 22, and the annular plate portion 22b is fixed to the flange portion 22d of the cylindrical portion 22a with a bolt 26 (see FIGS. 2 and 3). . As a result, the sample 10 can rotate around the first rotation axis C1.

  Next, as shown in FIG. 1, the sample rotating device 2 is placed and fixed on the movable stage 52 of the goniometer stage 5 (step S2). At that time, the sample rotation device 2 is fixed so that the first rotation axis C1 is disposed on the optical axis C0.

  Next, the goniometer stage 5 is driven to incline the first rotation axis C1 of the sample rotating device 2 by a predetermined acute angle θ with respect to the optical axis C0 in the above-described virtual plane (step S3, axis inclination step). . Specifically, the actuator of the goniometer stage 5 is driven, and the movable stage 52 is moved in a circular arc with respect to the fixed stage 51 by a predetermined amount in the y-axis direction (the positive direction of the y-axis in FIG. 1).

  Next, the rotation drive unit 23 of the sample rotation device 2 is driven, and the sample rotation unit 22 is rotated around the first rotation axis C1 together with the sample 10 with respect to the main body unit 21 (step S4, rotation process). Then, X-rays are emitted from the X-ray source 3, and the rotating sample 10 is irradiated with X-rays (step S5, irradiation process). Then, the diffracted X-ray 12 transmitted through the sample 10 and diffracted to the front of the sample rotating device 2 is detected by the diffracted X-ray detector 4 (step S6, detection step).

<Sample observation area>
FIGS. 5A to 5D are explanatory diagrams showing observation regions of the sample 10 by the diffraction X-ray detection unit 4.
In FIG. 5A, in the X-ray diffraction measurement, an infinite number of reciprocal lattice points becomes a spherical shell 61 (hereinafter referred to as a reciprocal lattice spherical shell) defined by the radius of the reciprocal 1 / d of the surface interval d. . Of the reciprocal lattice spherical shell, only the intersection (debye ring) 63 with the Ewald sphere 62 defined by the radius of the reciprocal 1 / λ of the wavelength λ of the incident X-ray satisfies the diffraction condition. For this reason, X-ray diffraction is observed in the direction of the conical generating line 64 with the center of the Ewald sphere 62 as the apex with respect to the incident X-ray (optical axis C0).

  FIG. 5B is a view of the reciprocal lattice spherical shell 61 and the Debye ring 63 viewed from the optical axis C0 direction with respect to the stationary sample 10. In general, in a measurement method in which the diffracted X-ray detection unit is moved on an arc locus, only a part of the Debye ring 63 is observed. 65 only included.

Therefore, when the sample 10 is stationary, the number of particles satisfying the diffraction condition is small, and the X-ray diffraction measurement cannot be performed with high accuracy.
On the other hand, when the sample 10 is rotated, the reciprocal lattice points that can be observed on the reciprocal lattice spherical shell 61 are present on the curved surface swept by the line segment 65. The measurement accuracy can be improved.

FIG. 5C shows a case where the first rotation axis C1 of the sample rotating device 2 is coincident with the second rotation axis C2 of the diffraction X-ray detection unit 4, that is, the first rotation axis C1 is relative to the optical axis C0. FIG. 6 is a diagram illustrating an observation region by the diffraction X-ray detection unit 4 when the two are orthogonal to each other.
The observation region shown in FIG. 5C corresponds to the case of X-ray diffraction measurement in which a conventional glass capillary is rotated. In this case, the reciprocal lattice points that can be observed are a band-shaped observation region 67 (region indicated by hatching in the figure) that makes one round of the equator on the reciprocal lattice spherical shell 61, and the line segment shown in FIG. Compared to 65, the observation area can be greatly expanded.

  However, when measuring the plate-like sample 10 as in the present embodiment, the first rotation axis C1 is used as the second rotation axis of the diffraction X-ray detection unit 4 as in X-ray diffraction measurement in which the glass capillary is rotated. Cannot match C2. Therefore, in the present embodiment, the first rotation axis C1 is tilted with respect to the optical axis C0 in order to expand the observation region by the diffraction X-ray detection unit 4.

  FIG. 5D is a diagram illustrating an observation region of the sample 10 by the diffraction X-ray detection unit 4 of the present embodiment. As shown in FIG. 5D, since the first rotation axis C1 of the present embodiment is inclined with respect to the optical axis C0, the observable reciprocal lattice point is more than the equator portion on the reciprocal lattice spherical shell 61. A band-shaped observation region 68 (region indicated by hatching in the figure) is formed so as to include a position where the latitude is slightly shifted. Although this observation region 68 is smaller than the observation region 67 shown in FIG. 5C, it can be seen that the observation region 68 is significantly larger than the line segment 65 shown in FIG. 5B.

<Verification experiment>
Next, a verification experiment performed by the present inventors in order to verify the effect obtained by the X-ray diffraction measurement apparatus 1 of the present embodiment will be described.
As an experimental method of the verification experiment, fine powder Si used for powder X-ray diffraction was used as a sample, 111 diffraction lines thereof were repeatedly measured, and the diffraction intensity was obtained.

Samples were measured under the following three conditions.
Condition A: When the rotation axis of the sample is inclined 20 ° with respect to the optical axis (corresponding to this embodiment)
Condition B: When the rotation axis of the sample is not inclined with respect to the optical axis Condition C: When the sample is not rotated

  In the above repeated measurement, the incident light energy was changed so that the particles satisfying the diffraction condition in the sample changed for each measurement. For this reason, the fluctuation (variation) of the diffraction intensity in each measurement is caused by the fluctuation of the number of particles due to this diffraction, that is, the measurement accuracy. Therefore, if the diffraction intensity of each measurement is constant, it means that the measurement accuracy is high.

FIG. 6 is a graph showing the experimental results of this verification experiment. This graph shows the relationship between the number of X-ray diffraction measurements and the diffraction intensity under the above conditions A to C.
As shown in FIG. 6, it can be seen that the fluctuation of the diffraction intensity under the condition A is the smallest compared with the diffraction intensity under the other conditions B and C. In particular, when the conditions A and C are compared, the fluctuation in the diffraction intensity is significantly smaller in the condition A. By rotating the sample, the measurement accuracy is greatly improved compared to the measurement of the stationary sample. I understand that Further, even when the conditions A and B are compared, it can be seen from the graph that the fluctuation of the diffraction intensity is smaller in the condition A.

In the graph of FIG. 6, in order to quantitatively evaluate the fluctuation of the diffraction intensity, the standard deviation σ of the fluctuation of the diffraction intensity in each condition A to C is shown. The standard deviation σ indicates that the smaller the value, the higher the measurement accuracy.
As shown in FIG. 6, the standard deviation σ of condition B is 0.62%, the standard deviation σ of condition C is 2.2%, whereas the standard deviation σ of condition A is 0.41%. And shows the minimum value. That is, it can be seen that it is quantitatively shown that the measurement accuracy is the highest in the case of condition A. Moreover, in the case of condition A, it is possible to measure with an accuracy 1.5 times or more that of condition B, and with an accuracy of 5 times or more that of condition C, and the effect of this embodiment can be achieved. It really represents.

  Further, as shown in FIG. 6, the error (standard deviation) σ ′ due to the fluctuation of the number of measured photons, that is, photon statistics, is 0.31%, and the conditions A to B in the present verification experiment The value of the standard deviation σ of the fluctuation of the diffraction intensity of C is always greater than the value of the standard deviation σ ′ according to photon statistics. Among them, the standard deviation σ (0.41%) of the condition A shows a value very close to the standard deviation σ ′ (0.31%) according to the photon statistics. It can be seen that the measurement can be performed with the accuracy that is thinned to the maximum accuracy that can be reached.

<About effect>
As described above, according to the X-ray diffraction measurement device 1 and the X-ray diffraction measurement method of the present embodiment, when the sample 10 is irradiated with X-rays, the sample rotation device 2 rotates the sample 10 within a predetermined plane. The sample can be rotated by the same method as the measurement method for rotating the rotary table. For this reason, unlike the conventional measurement method of rotating a glass capillary, it is not necessary to finely crush the sample, so that the sample can be subjected to X-ray diffraction measurement in a desired shape.

  In addition, the sample rotation device centered on the sample 10 rotated by the sample rotation device 2 in a virtual plane including the optical axis C0 of the X-ray and the second rotation axis C2 of the diffraction X-ray detection unit 4 by the axis tilt mechanism 5. The second first rotation axis C1 can be inclined at a predetermined acute angle θ with respect to the optical axis C0. Thereby, compared with the case where the 1st rotation axis C1 is not inclined with respect to the optical axis C0, the observation area | region of the sample 10 by the diffraction X-ray detection part 4 can be expanded. As a result, the number of particles satisfying the diffraction condition can be increased, so that the measurement accuracy of the X-ray diffraction measurement can be improved.

  Further, since the X-ray diffraction measurement apparatus 1 of the present embodiment uses a transmission method that detects the diffracted X-rays 12 that have been transmitted through the sample 10 and diffracted, a combination of X-ray diffraction measurement and X-ray absorption spectroscopy measurement. DAFS (Diffraction Anomalous Fine Structure) method and various X-ray resonance scattering measurements can be easily performed. Furthermore, if an X-ray diffraction measurement apparatus 1 is combined with an electrode rotation mechanism such as a slip ring, it is possible to perform measurement in situ while applying a voltage to the measurement sample.

In addition, since the shaft tilt mechanism 5 can adjust the acute angle θ, the tilt angle (sharp angle) of the first rotation axis C1 with respect to the optical axis C0 can be appropriately adjusted according to the sample 10.
In addition, by setting the acute angle θ to an angle range of 15 to 20 °, the observation region of the sample 10 by the diffracted X-ray detector 4 is expanded as much as possible while suppressing the amount of X-ray absorption by the sample 10. be able to.

  The present invention is not limited to the above-described embodiment, and can be implemented with appropriate modifications. For example, the sample 10 of the above embodiment is formed in a plate shape, but may be formed in any other shape. Further, as the sample 10 to be measured, a tablet sample or a device sample such as a thin laminate cell can be used. In particular, when a tablet sample is used, even if the sample has a large amount of X-ray absorption, the amount of X-ray absorption is adjusted by making the sample into a tablet shape formed by mixing a diluent. It becomes possible. As a result, it is possible to perform accurate X-ray diffraction measurement with correction of X-ray absorption.

  In the shaft tilt mechanism 5 of the above embodiment, the first rotation axis C1 is tilted with respect to the optical axis C0. However, the optical axis C0 may be tilted with respect to the first rotation axis C1. Further, in the X-ray diffraction measurement apparatus 1 of the above embodiment, the second rotation axis C2 of the diffraction X-ray detection unit 4 is arranged in the vertical direction (z-axis direction), but is arranged in the horizontal direction (x-axis direction). You may do it. In this case, since the first rotation axis C1 is inclined with respect to the optical axis C0 on the horizontal plane (xy plane), the axis inclination mechanism 5 for inclining the first rotation axis C1 is replaced with a goniometer stage. What is necessary is just to comprise by the turntable etc. which rotate on a horizontal surface centering on an axial direction.

DESCRIPTION OF SYMBOLS 1 X-ray-diffraction measuring apparatus 3 X-ray source 4 Diffraction X-ray detection part 5 Axis tilt mechanism 10 Sample 12 Diffraction X-ray 22 Sample rotation part C0 Optical axis C1 First rotation axis C2 Second rotation axis f Circular locus θ Sharp angle

Claims (5)

A sample rotating unit that rotates the sample within a predetermined plane by rotating around a predetermined first rotation axis;
An X-ray source for irradiating the sample rotated by the sample rotating unit with X-rays;
A diffracted X-ray detector that detects a diffracted X-ray transmitted through the sample and diffracted by moving on an arc locus centering on a second rotation axis orthogonal to the optical axis of the X-ray;
In a virtual plane including the optical axis and the second rotation axis, the first rotation axis is relatively inclined at a predetermined acute angle with respect to the optical axis with the sample rotated by the sample rotation unit as a center. An axis tilting mechanism,
An X-ray diffraction measurement apparatus comprising:   The X-ray diffraction measurement apparatus according to claim 1, wherein the shaft tilt mechanism is capable of adjusting the acute angle.   The X-ray diffraction measurement apparatus according to claim 1, wherein the acute angle is set in an angle range of 15 to 20 °.   The X-ray diffraction measurement apparatus according to claim 1, wherein the sample has a tablet shape. A rotating step of rotating the sample within a predetermined plane by rotating the sample rotating unit around a predetermined first rotation axis;
An irradiation process in which an X-ray source irradiates the sample rotated by the sample rotating unit with X-rays;
A detection step in which the diffracted X-ray detector detects a diffracted X-ray transmitted through the sample and diffracted by moving on an arc locus centering on a second rotation axis orthogonal to the optical axis of the X-ray. When,
The axis tilt mechanism has a predetermined acute angle with respect to the optical axis with respect to the optical axis about the sample rotated by the sample rotating part in a virtual plane including the optical axis and the second rotational axis. An axial tilting process for relatively tilting at
An X-ray diffraction measurement method comprising:

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