X-ray diffraction apparatus and measurement method

The X-ray diffractometer optimizes slit and detector alignment to enhance intensity and accuracy in X-ray diffraction measurements, addressing the limitations of existing technologies.

JP7868888B2Active Publication Date: 2026-06-02RIGAKU CORP

Patent Information

Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
RIGAKU CORP
Filing Date
2025-05-14
Publication Date
2026-06-02

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Abstract

To provide an X-ray diffraction device.SOLUTION: An X-ray diffraction device 100 comprises: an X-ray source 110; a sample table 130; a detector 160; and a slit member 150. The X-ray source is configured to be able to irradiate a sample F with an X-ray. The sample table is configured to be able to install the sample in such a way that the X-ray diffracts. The detector is configured to be able to detect a diffraction X-ray 140 serving as a diffracted X-ray in one dimension at a detection strip 161. The slit member is provided between the sample table and the detector, and has a slit 151 that allows the diffraction X-ray to pass through, and an axis in a longitudinal direction of the slit is parallel with an axis in a longitudinal direction of the detection strip.SELECTED DRAWING: Figure 1
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Description

[Technical Field]

[0001] The present invention relates to an X-ray diffraction apparatus and a measurement method. [Background technology]

[0002] Patent Document 1 discloses an X-ray diffraction apparatus that detects X-rays via a parallel slit analyzer. Patent Document 2 discloses an X-ray diffraction apparatus that detects diffracted X-rays using a one-dimensional detector, a two-dimensional detector, etc. [Prior art documents] [Patent Documents]

[0003] [Patent Document 1] Japanese Patent Publication No. 2007-010486 [Patent Document 2] Japanese Patent Publication No. 2020-153724 [Overview of the project] [Problems that the invention aims to solve]

[0004] However, in X-ray diffraction measurements that detect X-rays via a parallel slit analyzer (i.e., a PSA) such as the one described in Patent Document 1, it is difficult to maintain high accuracy and high intensity profiles, and there is still room for improvement.

[0005] Furthermore, even in X-ray diffraction measurements that do not use PSA, such as in Patent Document 2, accuracy and precision could not be maintained depending on the sample setup conditions, sample shape, etc., and there was still room for improvement.

[0006] The present invention was made to solve these problems, and in view of the above circumstances, aims to provide an X-ray diffraction apparatus and measurement method that can acquire highly accurate and precise profiles with higher intensity, regardless of conditions. [Means for solving the problem]

[0007] According to one aspect of the present invention, an X-ray diffractometer is provided. This X-ray diffractometer includes an X-ray source, a sample stage, a detector, and a slit member. The X-ray source is configured to irradiate the sample with X-rays. The sample stage is configured to be able to install a sample so that the X-rays are diffracted. The detector is configured to be able to detect one-dimensionally diffracted X-rays, which are the diffracted X-rays, with a detection strip. The slit member is provided between the sample stage and the detector. It has a slit through which the diffracted X-rays can pass. The longitudinal axis of the slit is parallel to the longitudinal axis of the detection strip.

Brief Description of the Drawings

[0008] [Figure 1] It is a side view showing an example of the X-ray diffractometer 100 according to Embodiment 1. [Figure 2] It is a diagram for explaining the relationship between the X-ray diffractometer 100 and the intensity of the profile. [Figure 3] It is a diagram for explaining each parameter of the X-ray diffractometer 100. [Figure 4] It is a diagram for explaining the relationship between the X-ray diffractometer 100 and the accuracy of the peak. [Figure 5] It is a side view for explaining an example of the relationship between the X-ray detection position D on the detection surface 160a of the detector 160 when the goniometer angle 2Θ and the diffraction angle 2θ coincide. [Figure 6] It is a perspective view for explaining an example of the relationship between the X-ray detection position D of the detector 160 when the goniometer angle 2Θ and the diffraction angle 2θ coincide. [Figure 7] It is a perspective view for explaining an example of the relationship between the X-ray detection position D on the detection surface 160a of the detector 160 when the goniometer angle 2Θ and the diffraction angle 2θ do not coincide. [Figure 8] It is a perspective view for explaining an example of the relationship between the X-ray detection position D on the detection surface 160a of the detector 160 when the goniometer angle 2Θ and the diffraction angle 2θ do not coincide. [Figure 9] It is a diagram for explaining the profile obtained by X-ray diffraction measurement. [Figure 10]This diagram illustrates the operation of the X-ray diffractometer 100 when acquiring data at the same diffraction angle 2θ. [Figure 11] This is a side view showing an example of the operation of the X-ray diffraction apparatus 100 according to Embodiment 1. [Figure 12] This is a side view showing an example of the operation of the X-ray diffraction apparatus 100 according to Embodiment 1. [Figure 13] This is a side view showing an example of an X-ray diffractometer 200 according to Comparative Example 1. [Figure 14] This is a side view showing an example of an X-ray diffractometer 300 according to Comparative Example 2. [Figure 15] This is an example of a diagram illustrating the accuracy and precision in X-ray diffraction measurements. [Figure 16] This figure shows an example of the results measured using each X-ray diffractometer 100, 200, and 300. [Figure 17] This figure shows an example of measurement results obtained by moving the sample F vertically using the X-ray diffractometer 100 in Embodiment 1. [Figure 18] This figure shows an example of measurement results obtained by moving the sample F vertically using the X-ray diffractometer 200 in Comparative Example 1. [Figure 19] This figure shows an example of the measurement results obtained by moving the sample F vertically using the X-ray diffractometer 300 in Comparative Example 2. [Figure 20] This figure shows an example of measurement results obtained by rotating the sample surface in the tilting direction using the X-ray diffractometer 100 in Embodiment 1. [Figure 21] This figure shows an example of measurement results obtained by rotating the sample surface in the tilting direction using the X-ray diffractometer 200 in Comparative Example 1. [Figure 22] This figure shows an example of measurement results obtained by rotating the sample surface in the tilting direction using the X-ray diffractometer 300 in Comparative Example 2. [Figure 23] This figure shows an example of measurement results when the beam width of the incident X-ray 120 is changed using the X-ray diffractometer 100 in Embodiment 1. [Figure 24]This figure shows an example of measurement results when the beam width of the incident X-ray 120 is changed using the X-ray diffractometer 200 in Comparative Example 1. [Figure 25] This figure shows an example of measurement results when the beam width of the incident X-ray 120 was changed using the X-ray diffractometer 300 in Comparative Example 2. [Figure 26] This figure shows an example of measurement results obtained by changing the incident angle of the incident X-rays 120 using the X-ray diffractometer 100 in Embodiment 1. [Figure 27] This figure shows an example of measurement results obtained by changing the incident angle of the incident X-rays 220 using the X-ray diffractometer 200 in Comparative Example 1. [Figure 28] This figure shows an example of measurement results obtained by changing the incident angle of the incident X-rays using the X-ray diffractometer 300 in Comparative Example 2. [Figure 29] This is a side view showing an example of an X-ray diffractometer 400 according to a modified example 1 of Embodiment 1. [Figure 30] This is a top view showing an example of an X-ray diffractometer 400 according to a modified example 1 of Embodiment 1. [Figure 31] This is a side view showing an example of an X-ray diffractometer 500 according to a modified example 2 of Embodiment 1. [Figure 32] This is a side view showing an example of an X-ray diffractometer 600 according to a modified example 3 of Embodiment 1. [Figure 33] This is a side view showing an example of an X-ray diffractometer 700 according to a modified example 4 of Embodiment 1. [Figure 34] This is a side view showing an example of an X-ray diffractometer 800 according to a modified example 5 of Embodiment 1. [Figure 35] This is a magnified view of the area enclosed by the dashed line in Figure 34. [Figure 36] This is a perspective view showing an example of an X-ray diffraction apparatus 900 according to Embodiment 2. [Figure 37] This is a perspective view showing an example of an X-ray diffractometer 1000 using a pinhole member 1050 and a two-dimensional detector 1060. [Modes for carrying out the invention]

[0009] The X-ray diffractometer according to the present invention will be described below based on embodiments. The various features shown in the embodiments below can be combined with each other. The present invention is not limited to these embodiments. In addition, in the drawings attached to this specification, components may be shown in different proportions than the actual ones in order to make characteristic parts easier to understand. In this specification, the three mutually orthogonal spatial axes are referred to as the X-axis, Y-axis, and Z-axis, and the directions along the X-axis, Y-axis, and Z-axis are referred to as the X-axis direction, Y-axis direction, and Z-axis direction, respectively. The same applies to the A-axis direction, B-axis direction, and C-axis direction.

[0010] X-ray diffraction measurement methods include out-of-plane and in-plane measurements, which are defined by the orientation of the lattice plane being measured. Out-of-plane measurement is a method for evaluating lattice planes that are not perpendicular to the surface of the sample, as shown in Figure 1. On the other hand, in-plane measurement is a method for evaluating lattice planes perpendicular to the surface of the sample, as shown in Figure 36, which will be described later.

[0011] [Embodiment 1] First, let's explain how to perform out-of-plane measurements. Figure 1 is a side view showing an example of an X-ray diffraction apparatus 100 according to Embodiment 1. The X-ray diffractometer 100 comprises an X-ray source 110, a sample stage 130, a slit member 150, and a detector 160. The X-ray source 110 is configured to irradiate the sample F with incident X-rays 120. The X-ray diffractometer 100 is a device for performing out-of-plane measurements.

[0012] The XYZ coordinate system in Figure 1 is a Cartesian coordinate system set with reference to the mounting surface 130a of the sample stage 130 where the sample F is placed. The positive and negative signs of the axes are as shown in the figure. The planes defined by the X and Y axes are parallel to the mounting surface 130a of the sample stage 130, and the Z axis is perpendicular to the mounting surface 130a of the sample stage 130. The same applies to the X, Y, and Z axes in the subsequent side views. Note that if a small amount of sample F is leveled on the mounting surface 130a, its thickness becomes negligibly small, so the sample surface can be treated as coinciding with the mounting surface 130a. In Embodiment 1, the XYZ coordinate system is based on the mounting surface 130a of the sample stage 130, but it can also be based on the sample surface.

[0013] Furthermore, the ABC coordinate system in Figure 1 is a Cartesian coordinate system set with reference to the detection surface 160a of the detector 160. The positive and negative signs of the axes are as shown in the figure. The planes defined by the A-axis and B-axis directions are parallel to the detection surface 160a of the detector 160, and the C-axis direction is perpendicular to the detection surface 160a of the detector 160. The same applies to the A-axis, B-axis, and C-axis directions in the subsequent side views.

[0014] In X-ray diffraction measurements, the detector 160 rotates and moves along a circle called the goniometer circle, with the goniometer center G as the reference point, in order to detect the X-rays diffracted by the sample F.

[0015] The X-ray source 110 irradiates the sample F on the sample stage 130 with incident X-rays 120. At this time, the X-rays irradiated from the X-ray source 110 onto the sample F are made into parallel X-rays by passing through an incident-side slit (not shown), etc. The X-ray source 110 may also be fixed so as to operate with reference to the center G of the goniometer. Furthermore, the X-ray source 110 may be configured to irradiate incident X-rays 120 consisting of characteristic X-rays such as CuKα and FeKα.

[0016] The sample stage 130 is configured to allow the sample F to be placed so that the incident X-rays 120 (X-rays) are diffracted. The sample F may be bonded to the sample stage 130. The surface of the sample F is irradiated with incident X-rays 120. The incident X-rays 120 emitted from the X-ray source 110 strike the surface of the sample F and are diffracted at a specific crystal lattice plane within the sample F. The diffracted X-rays 140 diffracted at the crystal lattice plane pass through the slit 151 of the slit member 150 and are detected by the detection strip 161 of the detector 160.

[0017] The slit member 150 is provided between the sample stage 130 and the detector 160. Here, the slit member 150 has a slit 151 through which diffracted X-rays 140 can pass. The longitudinal axis (B-axis direction) of the slit 151 of the slit member 150 is parallel to the longitudinal axis (B-axis direction) of the detection strip 161. That is, the slit 151 is formed along the B-axis direction. Also, the width of the slit 151 in the short direction (A-axis direction) is wider than the width of the detection strip 161 in the short direction (A-axis direction). In other embodiments, the width of the slit 151 in the short direction may be narrower than the width of the detection strip 161 in the short direction. Furthermore, the width of the slit 151 in the short direction may be equal to the width of the detection strip 161 in the short direction. Also, the slit 151 has a tapered shape in the direction from the sample stage 130 toward the detector 160. That is, the slit 151 has a tapered shape that widens in the + direction of the C-axis. By configuring the slit 151 in a tapered shape, the background of the profile can be reduced. The slit member 150 is supported on the sample stage 130, the detector 160, or the arm of the goniometer. Furthermore, the slit member 150 can be made of any material that does not transmit X-rays, such as molybdenum.

[0018] Furthermore, instead of irradiating an extremely small area with X-rays, a slit member 150 having a slit 151 of an appropriate size can be provided. This makes it possible to measure the X-rays diffracted from a specific position.

[0019] The detector 160 is configured to detect diffracted X-rays 140, which are diffracted X-rays, in one dimension using a detection strip 161. That is, the detector 160 is a one-dimensional position-sensitive detector in a plane parallel to the diffraction plane. The detection strip 161, which is configured as an elongated surface extending in the B-axis direction, constitutes one detection channel, and a large number of these detection channels (for example, 128) are arranged horizontally (A-axis direction) to form a detection surface 160a. When diffracted X-rays at an arbitrary diffraction angle 2θ are detected on the detection surface 160a, a high-intensity profile (peak) can be obtained by integrating the measurement results of the same diffraction angle 2θ measured by different detection strips 161. Here, the narrower the width of the detection strip 161, the higher the accuracy, but the lower the intensity. Also, by increasing the number of detection strips 161, high-intensity data can be obtained while maintaining high accuracy. Note that the detector 160 only needs to be capable of one-dimensional detection, and may also have the functionality to detect in zero or two dimensions.

[0020] Next, the relationship between the X-ray diffractometer 100 of this embodiment and the resulting profile will be explained using Figures 2 to 4. Figure 2 illustrates the relationship between the X-ray diffractometer 100 and the profile intensity. The shortest distance L from the sample F (more specifically, the center G of the goniometer) to the front surface 150a of the slit member 150. S and the slit width W in the short direction (A-axis direction) of slit 151 S This affects the intensity of the profile being measured. That is, as shown in Equation 1, the intensity of the measurable profile is given by the distance L. S and slit width W S It is proportional to the distance L. S By shortening the parameter, the profile strength can be increased without sacrificing accuracy.

[0021]

number

[0022] The shortest distance L from the center G of the goniometer to the front surface 150a of the slit member 150. S For example, the range is 5 to 160 mm, preferably 5 to 50 mm, specifically for example 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42 ,43,44,45,46,47,48,49,50,51,52,53,54,55,56,57,58,59,60,61,62,63,64,65,66,67,68,69,70,71,72,73,74,75,76,77,78,79,80,81,82,83,84,85,86,87,88,89,90,91,92 ,93,94,95,96,97,98,99,100,101,102,103,104,105,106,107,108,109,110,111,112,113,114,115,116,117,118,119,120,121,122,123,124,125,126,127,128,129,130,131, These are 132, 133, 134, 135, 136, 137, 138, 139, 140, 141, 142, 143, 144, 145, 146, 147, 148, 149, 150, 151, 152, 153, 154, 155, 156, 157, 158, 159, and 160 mm, and may also be within the range of any two of the values ​​exemplified here.

[0023] Also, the slit width W in the short direction (A-axis direction) of slit 151. Sis, for example, 0.01 to 3 mm, preferably any value between any two of the values exemplified here: 0.01, 0.02, 0.03, 0.04, 0.05, 0.06, 0.07, 0.08, 0.09, 0.1, 0.11, 0.12, 0.13, 0.14, 0.15, 0.16, 0.17, 0.18, 0.19, 0.2, 0.21, 0.22, 0.23, 0.24, 0.25, 0.26, 0.27, 0.28, 0.29, 0.3, 0.31, 0.32, 0.33, 0.34, 0.35, 0.36, 0.37, 0.38, 0.39, 0.4, 0.41, 0.42, 0.43, 0.44, 0.45, 0.46, 0.47, 0.48, 0.49, 0.5, 0.51, 0.52, 0.53, 0.54, 0.55, 0.56, 0.57, 0.58, 0.59, 0.6, 0.61, 0.62, 0.63, 0.64, 0.65, 0.66, 0.67, 0.68, 0.69, 0.7, 0.71, 0.72, 0.73, 0.74, 0.75, 0.76, 0.77, 0.78, 0.79, 0.8, 0.81, 0.82, 0.83, 0.84, 0.85, 0.86, 0.87, 0.88, 0.89, 0.9, 0.91, 0.92, 0.93, 0.94, 0.95, 0.96, 0.97, 0.98, 0.99, 1, 1.05, 1.1, 1.15, 1.2, 1.25, 1.3, 1.35, 1.4, 1.45, 1.5, 1.55, 1.6, 1.65, 1.7, 1.75, 1.8, 1.85, 1.9, 1.95, 2, 2.05, 2.1, 2.15, 2.2, 2.25, 2.3, 2.35, 2.4, 2.45, 2.5, 2.55, 2.6, 2.65, 2.7, 2.75, 2.8, 2.85, 2.9, 2.95, 3 mm, and may also be within the range between any two of the values exemplified here.

[0024] Next, the relationship between the X-ray diffractometer 100 and the accuracy of the peaks in the profile will be described using FIGS. 3 and 4. FIG. 3 is a diagram for explaining each parameter of the X-ray diffractometer 100. The accuracy of the peak is the shortest distance L from the front surface 150a of the slit member 150 to the detection surface 160a of the detector 160, the slit width W in the short side direction (A-axis direction) of the slit 151 S and the strip width W in the short side direction (A-axis direction) of the detection strip 161. DIt depends on.

[0025] Figure 4 illustrates the relationship between the X-ray diffractometer 100 and the peak accuracy. The peak width at half maximum (FWHM) is used as an indicator of accuracy. The FWHM can be approximated as shown in Equation 2. That is, by increasing the shortest distance L from the front surface 150a of the slit member 150 to the detection surface 160a of the detector 160, or by increasing the slit width W in the short direction (A-axis direction) of the slit 151. S Alternatively, the strip width W in the short direction (A-axis direction) of the detection strip 161. D By reducing this value, the half-width (FWHM) can be reduced, improving the accuracy of the peak.

[0026]

number

[0027] The strip width W of the detection strip 161 in the short direction (A-axis direction). D For example, it may be less than 0.01 mm, but is preferably 0.01 to 0.5 mm, and more preferably 0.05 to 0.2 mm, specifically for example 0.01, 0.02, 0.03, 0.04, 0.05, 0.06, 0.07, 0.08, 0.09, 0.1, 0.11, 0.12, 0.13, 0.14, 0.15, 0.16, 0.17, 0.18, 0.19, 0.2, 0.21, 0 The ranges are 0.22, 0.23, 0.24, 0.25, 0.26, 0.27, 0.28, 0.29, 0.3, 0.31, 0.32, 0.33, 0.34, 0.35, 0.36, 0.37, 0.38, 0.39, 0.4, 0.41, 0.42, 0.43, 0.44, 0.45, 0.46, 0.47, 0.48, 0.49, and 0.5 mm, and the range may be any two of the values ​​exemplified here.

[0028] The shortest distance L from the front surface 150a of the slit member 150 to the detection surface 160a of the detector 160 is, for example, 50 to 300 mm, preferably 100 to 300 mm, specifically, for example, 50, 60, 70, 80, 90, 100, 110, 120, 130, 140, 150, 160, 170, 180, 190, 200, 210, 220, 230, 240, 250, 260, 270, 280, 290, 300 mm, and may be within the range of any two of the values ​​exemplified here.

[0029] Therefore, according to equation 1, for the strength of the profile, the shortest distance L from the center G of the goniometer to the front surface 150a of the slit member 150 is S and the slit width W in the short direction (A-axis direction) of slit 151 S This can be adjusted arbitrarily. Also, from Equation 2, for peak accuracy, the shortest distance L from the front surface 150a of the slit member 150 to the detection surface 160a of the detector 160, and the slit width W are used. S and the strip width W in the short direction (A-axis direction) of the detection strip 161 D This can be adjusted arbitrarily. That is, in this embodiment, the distance L S Distance L, slit width W S and strip width W D By adjusting this, the strength and precision can be adjusted as desired.

[0030] Next, referring to Figures 5 to 8, the relationship between the goniometer angle 2Θ, the detection strips 161, 162, and 163 located at the X-ray detection position D on the detection surface 160a of the detector 160, and the diffraction angle 2θ will be explained. This relationship can be applied, at least, when the incident X-rays 120 are parallel X-rays, but is not limited to this case. First, using Figures 5 and 6, the case where the X-ray detection position D=0 will be explained. Here, the goniometer center line GL is a straight line that passes through the goniometer center G and extends in the Y-axis direction. The slit center line SL is a straight line that passes through the center of the slit 151 in the short-side direction (A-axis direction) and extends in the B-axis direction. Furthermore, the detector center line DL is a straight line that passes through the position of the X-ray detection position D=0 of the detector 160 and extends in the B-axis direction. Note that the straight lines connecting any two points on the goniometer center line GL, the slit center line SL, and the detector center line DL are collinear. Figure 5 is a side view illustrating an example of the relationship between the detection surface 160a of the detector 160 and the X-ray detection position D when the goniometer angle 2Θ and the diffraction angle 2θ coincide. Figure 6 is a perspective view illustrating an example of the relationship between the X-ray detection position D of the detector 160 when the goniometer angle 2Θ and the diffraction angle 2θ coincide.

[0031] As shown in Figures 5 and 6, the goniometer center G, the slit center line SL passing through the center of the slit 151 in the short direction (A-axis direction), and the detection strip 161 are aligned in a straight line. Assume that diffracted X-rays 141, diffracted at a diffraction angle of 2θ from the sample surface 131 located at the goniometer center G, pass through the slit 151 of the slit member 150 and reach the detector 160 located at a distance L from the slit 151. Let the angle of the goniometer at that time be 2Θ0, and the X-ray detection position D of the detector 160 be D=0. That is, when the goniometer angle is 2Θ0, the detection strip 161 (first detection strip) of the detector 160 at the X-ray detection position D=0 can detect the diffracted X-rays 141 diffracted at a diffraction angle of 2θ.

[0032] Next, we will explain the case where the X-ray detection position D ≠ 0 using Figures 7 and 8. Figure 7 is a perspective view illustrating an example of the relationship between the detection surface 160a of the detector 160 and the X-ray detection position D when the goniometer angle 2Θ and the diffraction angle 2θ do not coincide. As shown in Figure 7, the goniometer angle 2Θ is greater than the diffraction angle 2θ by δ i When it is small, the diffracted X-rays 142 diffracted from the sample surface 132 at a diffraction angle of 2θ pass through the slit 151, and the X-ray detection position D=D of the detector 160 i The X-rays reach the detection strip 162 (second detection strip). That is, the goniometer center G, the slit center line SL passing through the center of the slit 151 in the short direction (A-axis direction), and the detection strip 162 are aligned in a straight line. Note that the X-ray detection position D = D i This is a position that takes a positive value relative to the X-ray detection position D=0.

[0033] Figure 8 is a perspective view illustrating an example of the relationship between the detection surface 160a of the detector 160 and the X-ray detection position D when the goniometer angle 2Θ and the diffraction angle 2θ do not coincide. As shown in Figure 8, the goniometer angle 2Θ is greater than the diffraction angle 2θ by δ j When it is large, the diffracted X-rays 143 diffracted from the sample surface 133 at a diffraction angle of 2θ pass through the slit 151, and the X-ray detection position D=D of the detector 160 j The X-rays reach the detection strip 163 (second detection strip). That is, the goniometer center G, the slit center line SL passing through the center of the slit 151 in the short direction (A-axis direction), and the detection strip 163 are aligned in a straight line. Note that the X-ray detection position D = D j This is a position that takes a negative value relative to the X-ray detection position D=0.

[0034] The relationship shown in Equation 3 holds between the goniometer angle 2Θ, the diffraction angle 2θ, the X-ray detection position D of the detector 160, and the shortest distance L from the front surface 150a of the slit member 150 to the detection surface 160a of the detector 160. That is, the diffraction angle 2θ of the diffracted X-ray 141 depends on the shortest distance L from the front surface 150a of the slit member 150 to the detection surface 160a of the detector 160. From another perspective, the distance L between the front surface 150a of the slit member 150 and the detection surface 160a of the detector 160 depends on the diffraction angle 2θ of the diffracted X-ray 142, the goniometer angle 2Θ, and the shortest distance from the detection strip 161 (first detection strip) to the detection strip 162 (second detection strip).

[0035]

number

[0036] Figure 9 illustrates the profile obtained by X-ray diffraction measurement. The intensities obtained from each detection strip 161, 162, and 163 are integrated to form a profile. Specifically, first, the diffraction angle 2θ is calculated using Equation 3. For example, in Figure 6, the diffraction angle 2θ is calculated using the shortest distance L from the front surface 150a of the slit member 150 to the detection surface 160a of the detector 160, the goniometer angle 2Θ, and the X-ray detection position D=0. Also, in Figure 7, the distance L and the goniometer angle 2Θ are used. i and X-ray detection position D=D i The diffraction angle 2θ is calculated using this method. Furthermore, in Figure 8, the distance L and the goniometer angle 2Θ are shown. j and X-ray detection position D=D j By using this method, the diffraction angle 2θ is calculated. A profile can be obtained by integrating the intensity data obtained from each detection strip at the same diffraction angle 2θ. This allows the profile to be obtained using distance L as a parameter.

[0037] Next, the operation of the aforementioned X-ray diffractometer 100 will be explained. The X-ray source 110 irradiates the sample F on the sample stage 130 with incident X-rays 120, causing the X-rays to diffract. The diffracted X-rays 140 pass through the slit 151 of the slit member 150. The detector 160 detects the diffracted X-rays 140 in one dimension using the detection strip 161.

[0038] Figure 10 illustrates the operation of the X-ray diffractometer 100 when acquiring data at the same diffraction angle 2θ. In Figure 10, the slit member 150 and the detector 160 are in circular motion with respect to the goniometer center G. Specifically, the goniometer angle 2Θ and the X-ray detection position D change while the shortest distance L from the slit 151 to the detection surface 160a and the longitudinal axis (B-axis direction) of the slit 151 remain parallel to the longitudinal axis (B-axis direction) of the detection strip 161. When the diffraction angle 2θ of the diffracted X-ray 141 is equal to the goniometer angle 2Θ, the detector 160 detects the diffracted X-ray 142 with the detection strip 161 (first detection strip). When the diffraction angle 2θ is not equal to the goniometer angle 2Θ, the detector 160 detects the diffracted X-ray 142 and 143 with detection strips other than the detection strip 161 (first detection strip), such as 162, 163, etc. (second detection strip). In other words, even if the data is measured simultaneously (when the goniometer angle 2Θ is a predetermined value), the position of the detection strip will result in the measurement of data for a different diffraction angle 2θ.

[0039] Figure 11 is a side view showing an example of the operation of the X-ray diffraction apparatus 100 according to Embodiment 1. The sample stage 130 has a mounting surface 130a on which the sample F is placed, and moves parallel to the mounting surface 130a. That is, in Figure 11, the sample stage 130 moves in the X-axis direction (direction of the solid arrow) or the Y-axis direction. Such movement in the X-axis or Y-axis direction is effective in obtaining more accurate diffraction intensity when the particle size of the sample is non-uniform, etc. The sample stage 130 may also move perpendicular to the mounting surface 130a. That is, in Figure 11, the sample stage 130 can move in the Z-axis direction (direction of the dashed arrow). Furthermore, the sample stage 130 may be moved in the X-axis direction, Y-axis direction, or Z-axis direction without moving the incident side such as the X-ray source 110 or the light-receiving side such as the detector 160.

[0040] Figure 12 is a side view showing an example of the operation of the X-ray diffractometer 100 according to Embodiment 1. The sample stage 130 has a mounting surface 130a on which the sample F is placed, and is configured to allow the orientation of the mounting surface 130a to be changed. The sample stage 130 is configured to rotate around the X-axis (direction of the solid arrow) or the Y-axis (direction of the dashed arrow) with respect to the goniometer center G, in order to change the orientation of the mounting surface 130a. In this case, the sample stage 130 may be rotated only on the sample F without moving the incident side such as the X-ray source 110 or the light-receiving side such as the detector 160. In particular, for a sample F such as an epitaxial thin film whose lattice plane normal is oriented in a certain direction, if the angle between the lattice plane of the sample F and the incident X-ray 120 satisfies the diffraction condition when the sample F is rotated, the diffracted X-rays that satisfy that diffraction condition can be detected by the detection strip of the detector 160. In addition, the sample stage 130 may be configured to rotate around the Z-axis (direction of the dashed arrow) with respect to the goniometer center G without changing the orientation of the mounting surface 130a. The direction of rotation around the X-axis is also called the tilt direction.

[0041] [Comparative Example 1] Figure 13 is a side view showing an example of an X-ray diffractometer 200 according to Comparative Example 1. The X-ray diffractometer 200 of Comparative Example 1 comprises an X-ray source (not shown), a sample stage 230, a PSA 250, and a detector 260. For the basic configuration of the X-ray source, sample stage 230, and detector 260, please refer to the sample stage 130 and detector 160 of Embodiment 1. Note that the relationship between the diffraction angle 2θ and the goniometer angle 2Θ differs between Embodiment 1 and Comparative Example 1. Specifically, in the detector 160 of Embodiment 1, a certain goniometer angle 2Θ is converted to a diffraction angle 2θ based on the distance L from the front surface 150a of the slit member 150 to the detection surface 160a of the detector 160. However, in the detector 260 of Comparative Example 1, a certain goniometer angle 2Θ is treated as equal to the diffraction angle 2θ.

[0042] The PSA250 consists of multiple foils arranged in parallel. The detector 260 detects only the diffracted X-rays 240 that pass between the foils. This allows the detector 260 to acquire the same profile regardless of conditions such as the position of the sample stage 230. The accuracy of the PSA250 can be improved by narrowing the spacing between the foils and lengthening the optical path through the foils. However, when the spacing between the foils is narrowed, the diffracted X-rays may be scattered by the foils. The detection of these scattered diffracted X-rays reduces accuracy. Measurements using the PSA250 yield a profile with high accuracy but low intensity. Furthermore, even when the beam width of the diffracted X-rays widens, the resulting profile remains unchanged, enabling highly accurate measurements.

[0043] [Comparative Example 2] Figure 14 is a side view showing an example of an X-ray diffractometer 300 according to Comparative Example 2. The X-ray diffractometer 300 of Comparative Example 2 comprises an X-ray source (not shown), a sample stage 330, and a detector 360. For the X-ray source, sample stage 330, and detector 360, please refer to the sample stage 130 and detector 160 of Embodiment 1.

[0044] Next, we will explain the measurement results 1 to 5 for Embodiment 1, Comparative Example 1, and Comparative Example 2 described above.

[0045] [Measurement conditions] In the X-ray diffractometer 100 of Embodiment 1, the distance L between the goniometer center G and the front surface 150a of the slit member 150 is S The width is 30 mm. The distance L between the front surface 150a of the slit member 150 and the detection surface 160a of the detector 160 is 270 mm. Slit width W S The width is 0.15 mm. Strip width W D It is 0.1 mm. Furthermore, in the X-ray diffractometer 200 of Comparative Example 1, the aperture angle on the diagonal between the parallel foils of PSA250 (the acute angle in the region between the two dashed lines in Figure 13) is 0.114°. Furthermore, in the X-ray diffractometer 300 of Comparative Example 2, the distance between the goniometer center G and the detection surface 360a of the detector 360 is 300 mm, and the strip width is 0.1 mm.

[0046] Next, we will explain how to observe the profile obtained by X-ray diffraction measurement. Figure 15 is an example of a diagram illustrating accuracy and precision in X-ray diffraction measurements. In the profile obtained by X-ray diffraction measurement, peaks are observed. By analyzing the position and intensity of these peaks, the accuracy and precision of the sample can be determined. Accuracy is determined from the position of the peak. More specifically, accuracy is determined by the magnitude of the deviation between the reference position, where the peak should ideally be obtained, and the position of the actually measured peak. That is, if the position of the peak is close to the reference position, the accuracy can be judged as high. On the other hand, if the position of the peak is farther than the reference position, the accuracy can be judged as low. Precision is determined from the width of the peak (more specifically, the full width at half maximum, FWHM). More specifically, if the width of the peak is narrow, the precision can be judged as high. On the other hand, if the width of the peak is wide, the precision can be judged as low. Precision is also called angular precision.

[0047] [Measurement Results 1: Comparison of Intensities] Figure 16 shows an example of the results measured using each X-ray diffractometer 100, 200, and 300. In Figure 16, the solid line shows the measurement results with the slit member 150 of Embodiment 1. Also in Figure 16, the dashed line shows the measurement results using Comparative Example 1 with PSA 250. Furthermore, in Figure 16, the dashed line shows the measurement results of Comparative Example 2 without using a slit or PSA. Compared to the X-ray diffractometer 200 of Comparative Example 1 which uses PSA, the X-ray diffractometer 100 of Embodiment 1 shows higher peak intensity and narrower peak width, indicating that measurements can be performed with high intensity and high accuracy.

[0048] [Measurement result 2: Movement of the sample in the Z-axis direction] Next, we will explain the measurement results when the sample is moved vertically (in the Z-axis direction) using Figures 17 to 19. Figure 17 shows an example of measurement results obtained by moving the sample F vertically using the X-ray diffractometer 100 in Embodiment 1. Figure 18 shows an example of measurement results obtained by moving the sample F vertically using the X-ray diffractometer 200 in Comparative Example 1. Furthermore, Figure 19 shows an example of measurement results obtained by moving the sample F vertically using the X-ray diffractometer 300 in Comparative Example 2.

[0049] In Figures 17 to 19, the solid line shows the case where the sample F is placed at the center G of the goniometer. In Figures 17 to 19, the dashed line shows the case where the sample F is moved 0.5 mm upward from the center G of the goniometer. Furthermore, in Figures 17 to 19, the dashed line shows the case where the sample F is moved 0.5 mm downward from the center G of the goniometer.

[0050] As shown in Figure 17, in Embodiment 1 using the slit member 150, no shift in the peak position is observed even when the sample F moves, indicating high accuracy. On the other hand, as shown in Figure 18, in Comparative Example 1 using PSA250, although no shift in the peak position is observed when the sample F moves, indicating high accuracy, the precision is lower compared to Figure 17 because the accurate peak shape cannot be observed. Furthermore, as shown in Figure 19, in Comparative Example 2 without using a slit or PSA, a shift in the peak position is observed when the sample F moves, indicating a lack of accuracy. Furthermore, in temperature-variable measurements, the sample position may change vertically depending on the temperature, and in such cases, this embodiment proves to be effective.

[0051] [Measurement result 3: Changing the angle of the sample surface] Next, using Figures 20 to 22, we will explain the results of measurements taken by changing the direction of the sample surface (rotating around the X-axis). Figure 20 shows an example of measurement results obtained by rotating the sample surface in the tilting direction using the X-ray diffractometer 100 in Embodiment 1. Figure 21 shows an example of measurement results obtained by rotating the sample surface in the tilting direction using the X-ray diffractometer 200 in Comparative Example 1. Furthermore, Figure 22 shows an example of measurement results obtained by rotating the sample surface in the tilting direction using the X-ray diffractometer 300 in Comparative Example 2.

[0052] In Figures 20 to 22, the solid line shows the case where the tilt angle of the sample F is 0° relative to the goniometer center G. In Figures 20 to 22, the dashed line shows the case where the tilt angle of the sample F is 5° relative to the goniometer center G.

[0053] Figure 20 shows that in Embodiment 1 using the slit member 150, even when the sample surface is rotated in the tilting direction, the accurate peak shape is observed, and no shift in the peak position is observed, indicating high accuracy and precision. On the other hand, Figure 21 shows that in Comparative Example 1 using PSA 250, although the accuracy is high because no shift in the peak position is observed when the sample surface is rotated in the tilting direction, the accurate peak shape is not observed compared to Figure 20, indicating low precision. Furthermore, Figure 22 shows that in Comparative Example 2 without using a slit or PSA, although the accuracy is high because no shift in the peak position is observed when the sample surface is rotated in the tilting direction, the peak width is widened, indicating low precision. Furthermore, when measuring samples with uneven surfaces, the results will be affected in the same way as in this measurement. Therefore, even when measuring samples with uneven surfaces, it is effective to use the slit member 150.

[0054] [Measurement Result 4: Beam Width Change] Next, using Figures 23 to 25, we will explain the results of measurements taken by changing the beam width of the incident X-ray. Figure 23 shows an example of measurement results when the beam width of the incident X-ray 120 is changed using the X-ray diffractometer 100 in Embodiment 1. Figure 24 shows an example of measurement results when the beam width of the incident X-ray 120 is changed using the X-ray diffractometer 200 in Comparative Example 1. Furthermore, Figure 25 shows an example of measurement results when the beam width of the incident X-ray 120 is changed using the X-ray diffractometer 300 in Comparative Example 2.

[0055] In Figures 23 to 25, the solid line represents the case where the incident beam width is 0.8 mm. In Figures 23 to 25, the dashed line represents the case where the incident beam width is 0.4 mm. In Figures 23 to 25, the dashed line represents the case where the incident beam width is 0.1 mm.

[0056] As shown in Figure 23, in Embodiment 1 using the slit member 150, no change in peak shape is observed even when the beam width of the incident X-ray is changed, indicating that measurements can be taken with high accuracy. On the other hand, as shown in Figure 24, in Comparative Example 1 using the PSA250, when the beam width of the incident X-ray is changed, although the accurate peak shape cannot be observed at all compared to Figure 23, no change in peak shape is observed when the beam width of the incident X-ray is changed, so the impact on accuracy is small. Furthermore, as shown in Figure 25, in Comparative Example 2 without using a slit and PSA, when the beam width of the incident X-ray is changed, the peak width increases in proportion to the increase in the incident beam width, even though the peak has the same diffraction angle, indicating that the accuracy is low.

[0057] [Measurement Result 5: Change in Incident Angle of Incident X-rays] This section describes the results obtained by varying the angle of incidence of incident X-rays onto the sample. Figure 26 shows an example of measurement results obtained by changing the incident angle of incident X-rays 120 using the X-ray diffractometer 100 in Embodiment 1. Figure 27 shows an example of measurement results obtained by changing the incident angle of incident X-rays 220 using the X-ray diffractometer 200 in Comparative Example 1. Furthermore, Figure 28 shows an example of measurement results obtained by changing the incident angle of incident X-rays using the X-ray diffractometer 300 in Comparative Example 2.

[0058] In Figures 26 to 28, the solid lines show the results measured with a symmetrical arrangement (incident angle and exit angle are the same). In Figures 26 to 28, the dashed lines show the results when the incident angle is fixed at 1.0° and only the light-receiving side is moved during measurement.

[0059] As shown in Figure 26, in Embodiment 1 using the slit member 150, no change in the peak shape was observed when the incident angle of the incident X-rays was changed, indicating that measurements could be taken with high accuracy. On the other hand, as shown in Figure 27, in Comparative Example 1 using PSA, although no change in accuracy was observed when the incident angle of the incident X-rays was changed, the accurate peak shape could not be observed compared to Figure 26, indicating lower accuracy. As shown in Figure 28, in Comparative Example 2 without using a slit or PSA, when the incident angle of the incident X-rays was changed, the peak width increased despite the peak having the same diffraction angle, indicating a decrease in accuracy. Furthermore, when the incident angle is shallower than the exit angle, the beam width of the diffracted X-rays widens, resulting in the same condition as when the beam width of the incident X-rays was widened in measurement result 4. In in-plane measurements and measurements of thin film materials, measurements are sometimes performed with a small incident angle fixed relative to the sample surface, and it can be seen that this embodiment is effective in such cases.

[0060] Based on the above measurement results, Embodiment 1, which uses the slit member 150, yields higher accuracy and higher strength results compared to Comparative Example 1, which uses the PSA 250. Furthermore, the effects on accuracy and precision caused by changes in the sample position, the angle of tilt of the sample surface, the beam width of the incident X-ray, and the incident angle of the incident X-ray, which were observed in Comparative Example 2, which does not use a slit or PSA, were not observed in Embodiment 1.

[0061] [Example 1] Figure 29 is a side view showing an example of an X-ray diffractometer 400 according to Modification 1 of Embodiment 1. Figure 30 is a top view showing an example of an X-ray diffractometer 400 according to Modification 1 of Embodiment 1. The X-ray diffractometer 400 of the modified example 1 comprises an X-ray source (not shown), a sample stage 430, a slit member 450, a detector 460, and a monochromator 470. For the X-ray source, sample stage 430, and slit member 450, please refer to the sample stage 130 and slit member 150 of Embodiment 1.

[0062] The monochromator 470 has a grating surface that diffracts diffracted X-rays of a specific wavelength. Furthermore, the monochromator 470 is positioned between the slit member 450 and the detector 460, with the grating surface inclined from one end to the other in the longitudinal direction (B-axis direction) of the slit 451. Additionally, the monochromator 470 is positioned perpendicular to the diffraction angle. The monochromator 470 monochromatizes the diffracted X-rays. While graphite monochromators are primarily used for X-ray diffraction measurements using powder samples, the monochromator 470 is not limited to graphite.

[0063] The detector 460 is configured to detect diffracted X-rays of a specific wavelength diffracted by the monochromator 470. Specifically, the detector 460 is configured downstream of the monochromator 470, with its detection surface 460a facing the monochromator 470. Furthermore, the detector 460 is configured to be shifted in the Y-axis direction from the monochromator 470.

[0064] Next, we will explain the case where the incident X-rays are non-parallel using Figures 31 and 32. In particular, non-parallel incident X-rays 520 and 620 can be applied when the direction of propagation of the incident X-rays and the shape of the sample are known, except when the incident X-rays are focused by the sample.

[0065] [Differentiation 2] Figure 31 is a side view showing an example of an X-ray diffractometer 500 according to a modified example 2 of Embodiment 1. In the X-ray diffractometer 500 of the modified example 2, the X-ray source (not shown) irradiates the sample F with incident X-rays 520 so that they diverge in the direction of propagation.

[0066] [Difference 3] Figure 32 is a side view showing an example of an X-ray diffractometer 600 according to a modified example 3 of Embodiment 1. In the X-ray diffractometer 600 of the modified example 2, the X-ray source (not shown) irradiates the sample F with incident X-rays 620 so that they converge in the direction of propagation.

[0067] [Differentiation Example 4] Figure 33 is a side view showing an example of an X-ray diffractometer 700 according to a modified example 4 of Embodiment 1. In the X-ray diffractometer 700 of the modified example 4, a profile can be obtained while keeping the positions of the incident side, such as the X-ray source (not shown), the light-receiving side, such as the detector 760, and the sample stage 730 constant. In particular, it can be used when measuring changes over time using a powder sample F, when measuring peak changes at short time intervals such as during temperature-controlled measurements, or when simply measuring a narrow range (a single peak).

[0068] [Difference 5] Figure 34 is a side view showing an example of an X-ray diffractometer 800 according to a modified example 5 of Embodiment 1. The X-ray diffractometer 800 of the modified example 5 comprises an X-ray source (not shown), a sample stage 830, a slit member 850, a detector 860, and an interference prevention member 870. The sample stage 830 and detector 860 should be compared with the sample stage 130 and detector 160 of Embodiment 1.

[0069] The slit member 850 has a first slit 851 and a second slit 852. The longitudinal axis (B-axis direction) of the first slit 851 and the longitudinal axis (B-axis direction) of the second slit 852 are parallel.

[0070] The interference prevention member 870 is configured to prevent interference between the first diffracted X-ray 841 that has passed through the first slit 851 and the second diffracted X-ray 842 that has passed through the second slit 852, between the slit member 850 and the detector 860. In other words, the interference prevention member 870 extends from the slit member 850 toward the detector 860. To put it another way, the interference prevention member 870 extends in the C-axis direction. Furthermore, the interference prevention member 870 only needs to be made of a material that does not transmit X-rays, such as stainless steel. In addition, the shape of the interference prevention member 870 is not limited to a plate shape, as long as it is a shape that can shield X-rays so that diffracted X-rays that have passed through different slits do not interfere with each other. The interference prevention member 870 is also supported on the slit member 850, the detector 860, or the arm of the goniometer.

[0071] In modified example 5, there are two slits 851 and 852, but any number can be selected to expand the detection area of ​​the detector 860. Also, there is one interference prevention member 870, but any number can be selected to prevent interference between diffracted X-rays that have passed through different slits.

[0072] Next, with reference to Figure 35, the method for converting to a diffraction angle of 2θ when using the X-ray diffractometer 800 of Modified Example 5 will be explained. In Modified Example 5 as well, the diffraction angle 2θ of the diffracted X-rays 841 and 842 depends on the shortest distance L from the front surface 850a of the slit member 850 to the detection surface 860a of the detector 860. Figure 35 is an enlarged view of the area enclosed by the dashed line in Figure 34. The goniometer angle line AL is a straight line connecting the goniometer center G and the detector center line DL at the shortest distance. The slit center lines SL1 and SL2 are straight lines that pass through the center in the short direction (A-axis direction) of the slits 851 and 852 and extend in the B-axis direction. In the modified example 5, it is necessary to take into account the angle between the goniometer angle line AL and the line that connects the goniometer center G and the slit center line SL1 of the first slit 851 (and the slit center line SL2 of the second slit 852) in the shortest possible distance, convert it to a diffraction angle 2θ, and integrate the profile.

[0073] Here, the position of X-ray detection position D=0 is the position where the goniometer angle line AL and the detector 860 intersect, and is equal to the position of the detector center line DL. Distance S is the shortest distance from the slit center line SL1 of the first slit 851 (or the slit center line SL2 of the second slit 852) to the goniometer angle line AL. Furthermore, distance L is the distance from the front surface 850a of the slit member 850 to the detection surface 860a of the detector 860. From the above, the diffraction angle 2θ of the first diffracted X-ray detected at the X-ray detection position D=D1 after passing through the first slit 851 is expressed by the following equation 4. Also, the diffraction angle 2θ of the second diffracted X-ray 842 detected at the X-ray detection position D=D2 after passing through the second slit 852 is expressed by the following equation 5.

[0074]

number

[0075]

number

[0076] [Embodiment 2] The techniques disclosed herein can also be used for in-plane measurements. In-plane measurement allows for the direct measurement of diffraction from a lattice plane perpendicular to the surface of the sample, thus enabling direct evaluation of the structure near the surface and, as a result, accurate evaluation of the sample.

[0077] Figure 36 is a perspective view showing an example of an X-ray diffractometer 900 according to Embodiment 2. The X-ray diffractometer 900 of Embodiment 2 comprises an X-ray source (not shown), a sample stage 930, a slit member 950, and a detector 960. Specifically, the X-ray source irradiates the surface of the sample with incident X-rays 920 at a small incident angle onto the monochromatic, parallel surface of the sample. The incident X-rays 920 are diffracted by a lattice plane perpendicular to the sample surface, becoming diffracted X-rays 940 that travel in a direction just above the sample surface. These diffracted X-rays 940 are received by the detector 960 via the slit member 950. The detector 960 outputs an electrical signal corresponding to the intensity of the received X-rays.

[0078] Furthermore, in Embodiment 2, in order to detect the diffracted X-rays 940, the slit member 950 and the detector 960 are arranged such that the longitudinal directions of the slit 951 and the detection strip 961 are parallel. In addition to the X-ray diffractometer 900 that performs in-plane measurements, an in-plane reciprocal lattice mapping device or a GI-WAXS / SAXS (Grazing-IncidenceWide-AngleX-RayScattering / Small-AngleX-RayScattering) device can also be used.

[0079] [others] Furthermore, the techniques disclosed herein can also be used for measurements using pinhole and two-dimensional detectors. Figure 37 is a perspective view showing an example of an X-ray diffractometer 1000 using a pinhole member 1050 and a two-dimensional detector 1060. Embodiments 1 and 2 described the case using a slit and a one-dimensional detector, but Debye rings can also be detected instead of pinholes and two-dimensional detectors, respectively.

[0080] The X-ray diffractometer 1000 of this embodiment comprises an X-ray source (not shown), a sample stage 1030, a pinhole member 1050, and a two-dimensional detector 1060. The X-ray source irradiates the sample stage 1030 with incident X-rays 1020 parallel to it. A pinhole 1051 is formed in the center of the pinhole member 1050 to allow diffracted X-rays to pass through. Here, only the diffracted X-rays 1040 that pass through the pinhole 1051 from the X-rays diffracted by the crystal lattice planes perpendicular to the surface of the sample are directed towards the two-dimensional detector 1060. Furthermore, the two-dimensional detector 1060 detects the diffracted X-rays 1040 using pixels 1061, rather than detection strips that extend in the width direction like a one-dimensional detector. In another embodiment, multiple slit members may be provided between the sample stage 1030 and the two-dimensional detector 1060 so that the longitudinal directions of the slits are different for each, thereby serving as a substitute for the pinhole member 1050. For example, a first slit member whose longitudinal direction extends in the A-axis direction and a second slit member whose longitudinal direction extends in the B-axis direction may be provided between the sample stage 1030 and the two-dimensional detector 1060.

[0081] The technology disclosed herein relates to an X-ray diffractometer and measurement method using a slit (or pinhole) and a one-dimensional (or two-dimensional) detector, wherein the accuracy and precision of the peaks are independent of the sample position and shape. Furthermore, it is possible to obtain high-intensity and high-precision data compared to measurements using PSA. In addition, the intensity and precision can be selected by changing the slit position, slit width, and the arrangement of the slit and detector.

[0082] The product may be provided in any of the following embodiments. An X-ray diffractometer in which the slit has a tapered shape that widens from the sample stage toward the detector. An X-ray diffractometer in which the width of the slit in the short direction is wider than the width of the detection strip in the short direction. In the aforementioned X-ray diffractometer, the center of the goniometer circle, the center of the slit in the short direction, and the detection strip are arranged in a straight line. An X-ray diffractometer wherein the diffraction angle of the diffracted X-rays depends on the distance from the slit to the detector. An X-ray diffractometer in which the distance between the slit and the detector depends on the diffraction angle of the diffracted X-rays, the angle of the goniometer, and the distance from one detection strip to another detection strip. An X-ray diffractometer, wherein the detector detects the diffracted X-rays with a first detection strip when the diffraction angle of the diffracted X-rays is equal to the goniometer angle, and detects the diffracted X-rays with a second detection strip when the diffraction angle is not equal to the goniometer angle. An X-ray diffractometer comprising an interference prevention member, wherein the slit member has a first slit and a second slit, the longitudinal axis of the first slit and the longitudinal axis of the second slit are parallel, and the interference prevention member is configured to prevent interference between the first diffracted X-rays that have passed through the first slit and the second diffracted X-rays that have passed through the second slit between the slit member and the detector. An X-ray diffractometer comprising a monochromator, wherein the monochromator has a grating surface that diffracts the diffracted X-rays of a specific wavelength, and the grating surface is provided between the slit member and the detector at an inclination from one end to the other in the longitudinal direction of the slit. The X-ray diffractometer wherein the sample stage has a mounting surface on which the sample is placed and moves parallel to the mounting surface. An X-ray diffractometer wherein the sample stage has a mounting surface on which the sample is placed, and is configured to be rotatable around an axis so as to change the orientation of the mounting surface. An X-ray diffractometer in which the X-rays irradiated onto the sample from the X-ray source are parallel X-rays. A method for measuring a sample, wherein the sample is irradiated with X-rays, the X-rays are diffracted, the diffracted X-rays are passed through a slit, and the diffracted X-rays are detected in one dimension by a detection strip, the measurement method wherein the longitudinal axis of the slit is parallel to the longitudinal axis of the detection strip. Of course, this is not always the case.

[0083] Finally, while various embodiments relating to this disclosure have been described, these are presented as examples only and are not intended to limit the scope of the invention. These novel embodiments can be implemented in a variety of other forms, and various omissions, substitutions, and modifications can be made without departing from the spirit of the invention. These embodiments and their variations are included in the scope or spirit of the invention and in the scope of the invention and its equivalents as described in the claims. [Explanation of symbols]

[0084] 100: X-ray diffractometer 110:X-ray source 120: Incident X-ray 130: Sample stage 130a: Installation surface 131: Sample surface 132: Sample surface 133: Sample surface 140: Diffraction X-rays 141: Diffraction X-rays 142: Diffraction X-rays 143: Diffraction X-rays 150: Slit member 150a:Front 151: Slit 160: Detector 160a: Detection surface 161: Detection Strip 162: Detection Strip 163: Detection Strip 200: X-ray diffractometer 220: Incident X-ray 230: Sample stage 240: Diffraction X-rays 260: Detector 300: X-ray diffractometer 330: Sample stage 360: Detector 360a: Detection surface 400: X-ray diffractometer 430: Sample stage 450: Slit member 451: Slit 460: Detector 460a: Detection surface 470: Monochrometer 500: X-ray diffractometer 520: Incident X-ray 600: X-ray diffractometer 620: Incident X-ray 700: X-ray diffractometer 720: Incident X-ray 730: Sample stage 760: Detector 800: X-ray diffractometer 830: Sample stage 841: First Diffraction X-ray 842: Second Diffraction X-ray 850: Slit member 850a:Front 851: First slit 852: Second slit 860: Detector 860a: Detection surface 870: Interference prevention member 900: X-ray diffractometer 920: Incident X-ray 930: Sample stage 940: Diffraction X-rays 950: Slit member 951: Slit 960: Detector 961: Detection strip 1000: X-ray diffractometer 1020: Incident X-ray 1030: Sample stage 1040: Diffraction X-rays 1050: Pinhole component 1051: Pinhole 1060: 2D detector 1061: pixels 2Θ: Goniometer angle 2θ: diffraction angle AL: Goniometer square wire D: X-ray detection position DL: Detector centerline F: Sample G: Center of the goniometer GL: Goniometer centerline L: distance L S :distance S: distance SL: Slit centerline SL1: Slit centerline SL2: Slit centerline W D : Strip width W S : Slit width

Claims

1. An X-ray diffractometer, It comprises an X-ray source, a sample stage, a detector, and a pinhole member, The aforementioned X-ray source is configured to irradiate the sample with parallel X-rays, The sample stage is configured to allow the sample to be placed so that the parallel X-rays diffract. The detector is configured to detect the diffracted parallel X-rays, or diffracted X-rays, in two dimensions using pixels. The aforementioned pinhole member is Provided between the sample stage and the detector, Having a pinhole through which the diffracted X-rays can pass, X-ray diffractometer.

2. In the X-ray diffraction apparatus according to claim 1, The pinhole has a tapered shape that widens from the sample stage toward the detector. X-ray diffractometer.

3. In the X-ray diffraction apparatus according to claim 1 or claim 2, The center of the goniometer circle, the pinhole, and the pixel are aligned in a straight line. X-ray diffractometer.

4. In the X-ray diffraction apparatus according to claim 3, The diffraction angle of the diffracted X-rays depends on the distance from the pinhole to the detector. X-ray diffractometer.

5. In the X-ray diffraction apparatus according to claim 3 or claim 4, The distance between the pinhole and the detector depends on the diffraction angle of the diffracted X-rays, the angle of the goniometer, and the distance from one pixel to another. X-ray diffractometer.

6. In the X-ray diffractometer according to any one of claims 1 to 5, Equipped with an interference prevention member, The aforementioned pinhole member has a first pinhole and a second pinhole, The interference prevention member is configured to prevent interference between the first diffracted X-rays that have passed through the first pinhole and the second diffracted X-rays that have passed through the second pinhole, between the pinhole member and the detector. X-ray diffractometer.

7. In the X-ray diffraction apparatus according to any one of claims 1 to 6, Equipped with a monometer, The monochromator mentioned above is Having a lattice plane that diffracts the diffracted X-rays of a specific wavelength, A portion provided between the pinhole member and the detector, X-ray diffractometer.

8. An X-ray diffractometer, It comprises an X-ray source, a sample stage, a detector, and multiple slit members, The aforementioned X-ray source is configured to irradiate the sample with parallel X-rays, The sample stage is configured to allow the sample to be placed so that the parallel X-rays diffract. The detector is configured to detect the diffracted parallel X-rays, or diffracted X-rays, in two dimensions using pixels. The plurality of slit members are, Provided between the sample stage and the detector, Each has a slit through which the diffracted X-rays can pass, The longitudinal direction of each of the aforementioned slits is different. X-ray diffractometer.

9. In the X-ray diffraction apparatus according to claim 8, Each of the aforementioned slits has a tapered shape that widens from the sample stage toward the detector. X-ray diffractometer.

10. In the X-ray diffraction apparatus according to claim 8 or claim 9, The width of each of the aforementioned slits in the shorter direction is wider than the width of the aforementioned pixel. X-ray diffractometer.

11. In the X-ray diffraction apparatus according to any one of claims 8 to 10, The center of the goniometer circle, the center of each of the slits in the short direction, and the pixels are aligned in a straight line. X-ray diffractometer.

12. In the X-ray diffraction apparatus according to claim 11, The diffraction angle of the diffracted X-rays depends on the distance from the slit to the detector. X-ray diffractometer.

13. In the X-ray diffraction apparatus according to claim 11 or claim 12, The distance between the slit closest to the sample stage and the detector depends on the diffraction angle of the diffracted X-rays, the angle of the goniometer, and the distance from one pixel to another. X-ray diffractometer.

14. In the X-ray diffraction apparatus according to any one of claims 8 to 13, Equipped with an interference prevention member, Each of the aforementioned multiple slit members has a first slit and a second slit, The longitudinal axis of the first slit and the longitudinal axis of the second slit are parallel. The interference prevention member is configured to prevent interference between the first diffracted X-rays that have passed through the first slit and the second diffracted X-rays that have passed through the second slit, between the plurality of slit members and the detector. X-ray diffractometer.

15. In the X-ray diffractometer according to any one of claims 8 to 14, Equipped with a monometer, The monochromator mentioned above is Having a lattice plane that diffracts the diffracted X-rays of a specific wavelength, A device provided between the plurality of slit members and the detector, X-ray diffractometer.

16. In an X-ray diffractometer according to any one of claims 3 to 5 and claims 11 to 13, The detector detects the diffracted X-rays with a first pixel when the diffraction angle of the diffracted X-rays is equal to the goniometer angle, and detects the diffracted X-rays with a second pixel when the diffraction angle is not equal to the goniometer angle. X-ray diffractometer.

17. In an X-ray diffractometer according to any one of claims 1 to 16, The sample stage has a mounting surface on which the sample is placed, and moves parallel to the mounting surface. X-ray diffractometer.

18. In an X-ray diffraction apparatus according to any one of claims 1 to 17, The sample stage has a mounting surface on which the sample is placed, and is configured to be rotatable around an axis so as to change the orientation of the mounting surface. X-ray diffractometer.

19. A method for measuring a sample, The sample is irradiated with parallel X-rays, and the parallel X-rays are diffracted. The diffracted parallel X-rays, or diffracted X-rays, are passed through a pinhole. The sample is measured by detecting the diffracted X-rays in two dimensions using pixels. Measurement method.

20. A method for measuring a sample, The sample is irradiated with parallel X-rays, and the parallel X-rays are diffracted. The diffracted parallel X-rays, or diffracted X-rays, are passed through a plurality of slits. The sample is measured by detecting the diffracted X-rays in two dimensions using pixels. The longitudinal direction of each of the aforementioned slits is different. Measurement method.