X-ray diffraction device, and measurement method
The X-ray diffraction apparatus with a slit member and one-dimensional detector addresses precision and intensity challenges by optimizing slit and detection strip parameters, achieving high-precision and high-intensity profiles.
Patent Information
- Application Number
- JP2025081442
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2025-05-14
- Publication Date
- 2025-08-05
- Estimated Expiration
- 2042-02-14
AI Technical Summary
Existing X-ray diffraction measurements face challenges in maintaining high-precision and high-intensity profiles due to dependencies on sample installation conditions and sample shape, particularly when using a parallel slit analyzer (PSA), and there is a need for improved accuracy and precision regardless of these conditions.
An X-ray diffraction apparatus with a slit member having a slit parallel to the detection strip axis, allowing diffracted X-rays to pass through, combined with a one-dimensional detector, to achieve high-intensity and precise profiles by adjusting the distance and width of the slit and detection strip.
The apparatus enables high-intensity and high-precision X-ray diffraction measurements by optimizing the slit and detection strip parameters, enhancing accuracy and peak precision while maintaining intensity.
Smart Images

Figure 2025114821000001_ABST
Abstract
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 device that detects X-rays through a parallel slit analyzer, and Patent Document 2 discloses an X-ray diffraction device that detects diffracted X-rays using a one-dimensional detector, a two-dimensional detector, or the like. [Prior art documents] [Patent documents]
[0003] [Patent Document 1] Japanese Patent Application Laid-Open No. 2007-010486 [Patent Document 2] Japanese Patent Publication No. 2020-153724 Summary of the Invention [Problem to be solved by the invention]
[0004] However, in X-ray diffraction measurements in which X-rays are detected via a parallel slit analyzer (i.e., a PSA (Parallel Slit Analyzer)) as in Patent Document 1, it is difficult to maintain a high-precision and high-intensity profile, and there is still room for improvement.
[0005] Furthermore, even in X-ray diffraction measurements that do not use PSA, such as those in Patent Document 2, precision and accuracy cannot be maintained due to the dependency on sample installation conditions, sample shape, etc., and there is still room for improvement.
[0006] The present invention has been made to solve such problems, and in view of the above circumstances, it is an object of the present invention to provide an X-ray diffraction apparatus and measurement method that can obtain highly accurate and precise profiles at higher intensities regardless of conditions. [Means for solving the problem]
[0007] According to one aspect of the present invention, there is provided an X-ray diffraction device. The X-ray diffraction device includes an X-ray source, a sample stage, a detector, and a slit member. The X-ray source is configured to irradiate a sample with X-rays. The sample stage is configured to allow a sample to be placed thereon so that the X-rays are diffracted. The detector is configured to allow diffracted X-rays to be detected one-dimensionally by 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 explanation of the drawings]
[0008] [Figure 1] 1 is a side view showing an example of an X-ray diffraction apparatus 100 according to a first embodiment. [Figure 2] FIG. 2 is a diagram illustrating the relationship between the X-ray diffraction device 100 and the intensity of the profile. [Figure 3] FIG. 2 is a diagram illustrating each parameter of the X-ray diffraction apparatus 100. [Figure 4] FIG. 2 is a diagram illustrating the relationship between the X-ray diffraction apparatus 100 and peak accuracy. [Figure 5] 10 is a side view illustrating an example of the relationship between the goniometer angle 2Θ and the diffraction angle 2θ and 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 with each other. [Figure 6] 10 is a perspective view illustrating an example of the relationship between the goniometer angle 2Θ and the diffraction angle 2θ and the X-ray detection position D of the detector 160 when they coincide with each other. FIG. [Figure 7] 10 is a perspective view illustrating an example of the relationship between the goniometer angle 2Θ and the diffraction angle 2θ and the X-ray detection position D on the detection surface 160a of the detector 160 when they do not coincide with each other. FIG. [Figure 8] 10 is a perspective view illustrating an example of the relationship between the goniometer angle 2Θ and the diffraction angle 2θ and the X-ray detection position D on the detection surface 160a of the detector 160 when they do not coincide with each other. FIG. [Figure 9] FIG. 1 is a diagram illustrating a profile obtained by X-ray diffraction measurement. [Figure 10]10A and 10B are diagrams illustrating the operation of the X-ray diffraction apparatus 100 when acquiring data on the same diffraction angle 2θ. [Figure 11] 1 is a side view showing an example of the operation of the X-ray diffraction apparatus 100 according to the first embodiment. [Figure 12] 1 is a side view showing an example of the operation of the X-ray diffraction apparatus 100 according to the first embodiment. [Figure 13] 1 is a side view showing an example of an X-ray diffraction apparatus 200 according to Comparative Example 1. FIG. [Figure 14] 10 is a side view showing an example of an X-ray diffraction apparatus 300 according to Comparative Example 2. FIG. [Figure 15] 1 is an example of a diagram illustrating accuracy and precision in X-ray diffraction measurement. [Figure 16] 1A and 1B are diagrams showing examples of the results of measurements using the X-ray diffraction devices 100, 200, and 300. [Figure 17] 1 is a diagram showing an example of the results of measurements carried out by using the X-ray diffraction apparatus 100 in the first embodiment while moving the sample F in the vertical direction. [Figure 18] 10 is a diagram showing an example of the results of measurements carried out by using the X-ray diffraction apparatus 200 in Comparative Example 1 while moving the sample F in the vertical direction. FIG. [Figure 19] 10 is a diagram showing an example of the results of measurements carried out by using the X-ray diffraction apparatus 300 in Comparative Example 2 while moving the sample F in the vertical direction. FIG. [Figure 20] 1 is a diagram showing an example of the results of a measurement performed by rotating the surface of a sample in the tilt direction using the X-ray diffraction apparatus 100 in the first embodiment. [Figure 21] 10 is a diagram showing an example of the results of a measurement performed by rotating the surface of a sample in the tilt direction using the X-ray diffraction apparatus 200 in Comparative Example 1. FIG. [Figure 22] 10 is a diagram showing an example of the results of a measurement performed by rotating the surface of a sample in the tilt direction using the X-ray diffraction apparatus 300 in Comparative Example 2. FIG. [Figure 23] 10 is a diagram showing an example of the results of measurements when the beam width of incident X-rays 120 is changed using the X-ray diffraction apparatus 100 in the first embodiment. FIG. [Figure 24]10 is a diagram showing an example of the results of measurements when the beam width of the incident X-rays 120 is changed using the X-ray diffraction apparatus 200 in Comparative Example 1. FIG. [Figure 25] 10 is a diagram showing an example of the results of measurements when the beam width of the incident X-rays 120 is changed using the X-ray diffraction apparatus 300 in Comparative Example 2. FIG. [Figure 26] 1 is a diagram showing an example of the results of measurements performed by changing the incident angle of incident X-rays 120 using the X-ray diffraction apparatus 100 according to the first embodiment. [Figure 27] 10 is a diagram showing an example of the results of measurements carried out by changing the incident angle of incident X-rays 220 using the X-ray diffraction apparatus 200 in Comparative Example 1. FIG. [Figure 28] 10 is a diagram showing an example of the results of measurements carried out by changing the incident angle of incident X-rays using the X-ray diffraction apparatus 300 in Comparative Example 2. FIG. [Figure 29] 1 is a side view showing an example of an X-ray diffraction apparatus 400 according to a first modification of the first embodiment. [Figure 30] 1 is a top view showing an example of an X-ray diffraction apparatus 400 according to a first modification of the first embodiment. [Figure 31] 10 is a side view showing an example of an X-ray diffraction apparatus 500 according to a second modification of the first embodiment. FIG. [Figure 32] 10 is a side view showing an example of an X-ray diffraction apparatus 600 according to a third modification of the first embodiment. FIG. [Figure 33] 10 is a side view showing an example of an X-ray diffraction apparatus 700 according to a fourth modification of the first embodiment. FIG. [Figure 34] 10 is a side view showing an example of an X-ray diffraction apparatus 800 according to a fifth modification of the first embodiment. FIG. [Figure 35] FIG. 35 is an enlarged view of the area surrounded by the dashed line in FIG. 34. [Figure 36] FIG. 10 is a perspective view showing an example of an X-ray diffraction apparatus 900 according to a second embodiment. [Figure 37] 1 is a perspective view showing an example of an X-ray diffraction apparatus 1000 that uses a pinhole member 1050 and a two-dimensional detector 1060. FIG. DETAILED DESCRIPTION OF THE INVENTION
[0009] An X-ray diffraction apparatus according to the present invention will be described below based on an embodiment. The various features shown in the following embodiments can be combined with one another. However, the present invention is not limited to this embodiment. Furthermore, in the drawings attached to this specification, components may be shown at different scales than in reality in order to clearly show characteristic parts. Furthermore, in this specification, 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, Y-axis, and Z-axis directions, respectively. The same applies to the A-axis, B-axis, and C-axis directions.
[0010] X-ray diffraction measurement methods include out-of-plane measurement and in-plane measurement, each defined by the direction of the lattice plane being measured. Out-of-plane measurement is a method for evaluating lattice planes that are not perpendicular to the sample surface, as shown in Figure 1. On the other hand, in-plane measurement is a method for evaluating lattice planes that are perpendicular to the sample surface, as shown in Figure 36, which will be described later.
[0011] [Embodiment 1] First, the case where out-of-plane measurement is performed will be described. FIG. 1 is a side view showing an example of an X-ray diffraction apparatus 100 according to the first embodiment. The X-ray diffraction apparatus 100 includes 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 be able to irradiate incident X-rays 120 onto a sample F. The X-ray diffraction apparatus 100 is an apparatus that performs out-of-plane measurement.
[0012] The XYZ coordinate system in FIG. 1 is a Cartesian coordinate system set based on the mounting surface 130a of the sample stage 130 on which the sample F is mounted. The positive and negative axes are as shown. The plane defined by the X-axis and Y-axis directions is parallel to the mounting surface 130a of the sample stage 130, and the Z-axis direction is perpendicular to the mounting surface 130a of the sample stage 130. The same applies to the X-axis, Y-axis, and Z-axis directions in the subsequent side views. Note that when a trace amount of sample F is flattened on the mounting surface 130a, its thickness becomes negligibly small, so the sample surface can be treated as coinciding with the mounting surface 130a. Furthermore, although the XYZ coordinates in the first embodiment are based on the mounting surface 130a of the sample stage 130, they may also be based on the sample surface.
[0013] 1 is a Cartesian coordinate system set based on the detection surface 160a of the detector 160. The positive and negative directions of the axes are as shown. The plane defined by the A-axis and B-axis directions is 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 the X-ray diffraction measurement, the detector 160 rotates and moves along a circle called a goniometer circle, with the goniometer center G as the reference, in order to detect X-rays diffracted by the sample F.
[0015] The X-ray source 110 irradiates incident X-rays 120 toward a sample F on a sample stage 130. At this time, the X-rays irradiated from the X-ray source 110 to the sample F are converted into parallel X-rays by passing through an entrance-side slit (not shown), for example. The X-ray source 110 may also be fixed so as to operate based on the goniometer center G. 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 thereon so that incident X-rays 120 (X-rays) are diffracted. The sample F may be glued to the sample stage 130. The incident X-rays 120 are irradiated onto the surface of the sample F. The incident X-rays 120 emitted from the X-ray source 110 hit the surface of the sample F and are diffracted by a specific crystal lattice plane within the sample F. The diffracted X-rays 140 diffracted by the crystal lattice plane pass through a slit 151 in the slit member 150 and are detected by a detection strip 161 in 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 that allows the diffracted X-rays 140 to pass through. 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. Furthermore, the width of the slit 151 in the lateral direction (A-axis direction) is wider than the width of the detection strip 161 in the lateral direction (A-axis direction). In other embodiments, the width of the slit 151 in the lateral direction may be narrower than the width of the detection strip 161 in the lateral direction. Furthermore, the width of the slit 151 in the lateral direction may be equal to the width of the detection strip 161 in the lateral direction. Furthermore, the slit 151 has a tapered shape in a direction from the sample stage 130 toward the detector 160. That is, the slit 151 has a tapered shape that widens in the positive direction of the C-axis. The background of the profile can be reduced by configuring the slit 151 in a tapered shape. The slit member 150 is supported on the sample stage 130, the detector 160, or the arm of a goniometer. The slit member 150 may 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, which makes it possible to measure X-rays diffracted from a specific position.
[0019] The detector 160 is configured to detect diffracted X-rays 140, which are diffracted X-rays, one-dimensionally using the detection strips 161. That is, the detector 160 is a one-dimensional position-sensitive detector in a plane parallel to the diffraction plane. The detection strips 161, configured as elongated surfaces extending in the B-axis direction, constitute one detection channel, and a number of these detection channels (e.g., 128) are arranged horizontally (in the A-axis direction) to form the 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 accumulating the measurement results for the same diffraction angle 2θ measured by different detection strips 161. Here, the narrower the width of the detection strips 161, the higher the accuracy but the lower the intensity. Furthermore, by increasing the number of detection strips 161, high-intensity data can be obtained while maintaining high accuracy. Note that the detector 160 may be capable of one-dimensional detection and may also be capable of zero-dimensional or two-dimensional detection.
[0020] Next, the relationship between the X-ray diffraction apparatus 100 of this embodiment and the obtained profile will be described with reference to FIGS. FIG. 2 is a diagram illustrating the relationship between the X-ray diffraction device 100 and the intensity of the profile. The shortest distance L from the sample F (more specifically, the goniometer center G) to the front surface 150a of the slit member 150 S and the slit width W in the short direction (A-axis direction) of the slit 151 S affects the intensity of the measured profile. That is, as shown in Equation 1, the measurable profile intensity is S and slit width W S is proportional to the distance L S Shortening the θ will result in a stronger profile without sacrificing accuracy.
[0021]
number
[0022] The shortest distance L from the goniometer center G to the front surface 150a of the slit member 150 S is, for example, 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, 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, 160 mm, and may be within a range between any two of the values exemplified here.
[0023] In addition, the slit width W of the slit 151 in the short side direction (A axis direction) Sis, for example, 0.01 to 3 mm, and preferably 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 ,0.33,0.34,0.35,0.36,0.37,0.38,0.39,0.4,0.41,0.42,0.43,0.44,0.45,0.46,0.47,0.48,0.49,0.5,0.51,0.52,0.53,0.54,0.55,0.56,0.57,0.58,0.59,0.6,0.61,0.62,0.63,0.64,0.65,0.66,0.67,0.68,0.6 9,0.7,0.71,0.72,0.73,0.74,0.75,0.76,0.77,0.78,0.79,0.8,0.81,0.82,0.83,0.84,0.85,0.86,0.87,0.88,0.89,0.9,0.91,0.92,0.93,0.94,0.95,0.96,0.97,0.98,0.99,1,1.05,1.1,1.15,1.2,1.25,1.3,1. 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 be within a range between any two of the numerical values exemplified here.
[0024] Next, the relationship between the X-ray diffraction apparatus 100 and the accuracy of peaks in a profile will be described with reference to FIGS. FIG. 3 is a diagram illustrating each parameter of the X-ray diffraction apparatus 100. The accuracy of the peak is determined by the following relationship: 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 direction (A-axis direction) of the slit 151, S and the strip width W of the detection strip 161 in the short direction (A-axis direction) DDepends on.
[0025] FIG. 4 is a diagram illustrating the relationship between the X-ray diffraction apparatus 100 and peak accuracy. The full width half maximum (FWHM) of the peak is used as an index of accuracy. The full width half maximum (FWHM) can be approximated as shown in Equation 2. That is, the shortest distance L from the front surface 150a of the slit member 150 to the detection surface 160a of the detector 160 is increased, or the slit width W in the short direction (A-axis direction) of the slit 151 is increased. S Or the strip width W in the short direction (A-axis direction) of the detection strip 161 D By reducing the FWHM, the full width at half maximum (FWHM) can be reduced, and the accuracy of the peak can be improved.
[0026]
number
[0027] Strip width W of the detection strip 161 in the short direction (A-axis direction) D may be, for example, 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, 0.22, 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 mm, and may be within a range between 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, and 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, or 300 mm, and may be within a range between any two of the numerical values exemplified here.
[0029] Therefore, from Equation 1, for the strength of the profile, the shortest distance L from the goniometer center G 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 the slit 151 S is arbitrarily adjusted. Furthermore, from Equation 2, for the accuracy of the peak, 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 S and the strip width W of the detection strip 161 in the short direction (A-axis direction) D That is, in this embodiment, the distance L S , distance L, slit width W S and strip width W D By adjusting the value, the strength and precision can be adjusted arbitrarily.
[0030] Next, with reference to FIGS. 5 to 8 , the relationship between the goniometer angle 2Θ, the detection strips 161, 162, and 163 at the X-ray detection position D on the detection surface 160a of the detector 160, and the diffraction angle 2θ will be described. This relationship is applicable at least when the incident X-rays 120 are parallel X-rays, but is not limited to this. First, with reference to FIGS. 5 and 6 , the case where the X-ray detection position D=0 will be described. 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 direction (A-axis direction) and extends in the B-axis direction. The detector center line DL is a straight line that passes through the X-ray detection position D=0 of the detector 160 and extends in the B-axis direction. Note that the lines connecting any two points on the goniometer center line GL, the slit center line SL, and the detector center line DL are aligned. Fig. 5 is a side view illustrating 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 with each other. Fig. 6 is a perspective view illustrating an example of the relationship between the X-ray detection position D on the detector 160 when the goniometer angle 2Θ and the diffraction angle 2θ coincide with each other.
[0031] 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 arranged on a straight line. Assume that diffracted X-rays 141 diffracted at a diffraction angle 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 a distance L away from the slit 151. The goniometer angle at that time is 2Θ0, and the X-ray detection position D of the detector 160 is D=0. That is, when the goniometer angle is 2Θ0, the detection strip 161 (first detection strip) of the detector 160 located at the X-ray detection position D=0 can detect the diffracted X-rays 141 diffracted at a diffraction angle 2θ.
[0032] Next, the case where the X-ray detection position D≠0 will be described with reference to FIGS. FIG. 7 is a perspective view illustrating an example of the relationship between the goniometer angle 2Θ and the diffraction angle 2θ and the X-ray detection position D on the detection surface 160a of the detector 160 when they do not coincide with each other. As shown in Figure 7, the goniometer angle 2Θ is larger than the diffraction angle 2θ by δ i When the diffraction angle θ is small by 1 / 2, the diffracted X-ray 142 diffracted from the sample surface 132 at the diffraction angle 2θ passes through the slit 151 and reaches the X-ray detection position D=D of the detector 160. i 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 arranged on a straight line. Note that the X-ray detection position D=D i is a position that takes a positive value based on the X-ray detection position D=0.
[0033] FIG. 8 is a perspective view illustrating an example of the relationship between the goniometer angle 2Θ and the diffraction angle 2θ and the X-ray detection position D on the detection surface 160a of the detector 160 when they do not coincide with each other. As shown in Figure 8, the goniometer angle 2Θ is larger than the diffraction angle 2θ by δ j When the diffraction angle θ is larger than the diffraction angle θ, the diffracted X-ray 143 diffracted from the sample surface 133 passes through the slit 151 and reaches the X-ray detection position D=D of the detector 160. j 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 arranged on a straight line. Note that the X-ray detection position D=D j is a position that takes a negative value based on the X-ray detection position D=0.
[0034] The relationship shown in Expression 3 holds among 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-rays 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-rays 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] FIG. 9 is a diagram illustrating a profile obtained by X-ray diffraction measurement. The intensities obtained from each of the detection strips 161, 162, and 163 are integrated to form a profile. Specifically, first, the diffraction angle 2θ is calculated using Equation 3. For example, in FIG. 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 FIG. 7, the distance L, the goniometer angle 2θ, i and X-ray detection position D = D i Furthermore, in Figure 8, the distance L and the goniometer angle 2Θ are used to calculate the diffraction angle 2Θ. j and X-ray detection position D = D j The diffraction angle 2θ is calculated using the formula: For the intensity data obtained from each detection strip, a profile can be obtained by integrating the data at the same diffraction angle 2θ. This allows a profile to be obtained using the distance L as a parameter.
[0037] Next, the operation of the above-mentioned X-ray diffraction apparatus 100 will be described. The X-ray source 110 irradiates the sample F on the sample stage 130 with incident X-rays 120, causing the X-rays to be diffracted. The diffracted X-rays, or diffracted X-rays 140, pass through a slit 151 in the slit member 150. The detector 160 detects the diffracted X-rays 140 one-dimensionally with a detection strip 161.
[0038] FIG. 10 is a diagram illustrating the operation of the X-ray diffraction apparatus 100 when acquiring data for the same diffraction angle 2θ. In Figure 10, the slit member 150 and the detector 160 perform circular motion around the goniometer center G. Specifically, the goniometer angle 2Θ and the X-ray detection position D change while maintaining the shortest distance L from the slit 151 to the detection surface 160a and the longitudinal axis (B-axis direction) of the slit 151 parallel to the longitudinal axis (B-axis direction) of the detection strip 161. The detector 160 detects the diffracted X-rays 142 by the detection strip 161 (first detection strip) when the diffraction angle 2Θ of the diffracted X-rays 141 is equal to the goniometer angle 2Θ. When the diffraction angle 2Θ is not equal to the goniometer angle 2Θ, the detector 160 detects the diffracted X-rays 142 and 143 by detection strips 162, 163, etc. (second detection strips) other than the detection strip 161 (first detection strip). That is, even if the data are measured simultaneously (when the goniometer angle 2θ is a predetermined value), data for different diffraction angles 2θ are measured depending on the position of the detection strip.
[0039] FIG. 11 is a side view showing an example of the operation of the X-ray diffraction apparatus 100 according to the first embodiment. 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 FIG. 11, the sample stage 130 moves in the X-axis direction (the 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, for example. The sample stage 130 may also move perpendicular to the mounting surface 130a. That is, in FIG. 11, the sample stage 130 can move in the Z-axis direction (the direction of the dashed-dotted arrow). Furthermore, only the sample stage 130 may move in the X-axis, Y-axis, or Z-axis direction without moving the incident side of the X-ray source 110, etc. and the light-receiving side of the detector 160, etc.
[0040] FIG. 12 is a side view showing an example of the operation of the X-ray diffraction apparatus 100 according to the first embodiment. The sample stage 130 has a mounting surface 130a on which a sample F is placed, and the orientation of the mounting surface 130a is changeable. The sample stage 130 is rotatable about the X-axis (indicated by the solid arrow) or the Y-axis (indicated by the dashed arrow) around the goniometer center G so as to change the orientation of the mounting surface 130a. In this case, the sample stage 130 may rotate only the sample F without moving the incident side of the X-ray source 110 or the light-receiving side of the detector 160. In particular, for a sample F such as an epitaxial thin film whose lattice plane normal faces a fixed direction, if the angle between the lattice plane of the sample F and the incident X-ray 120 satisfies a diffraction condition by rotating the sample F, the diffracted X-rays that satisfy the diffraction condition can be detected by the detection strip of the detector 160. In addition, the sample stage 130 may be rotatable about the Z-axis (indicated by the dashed arrow) around the goniometer center G without changing the orientation of the mounting surface 130a. The rotation direction around the X-axis is also called the tilt direction.
[0041] [Comparative Example 1] FIG. 13 is a side view showing an example of an X-ray diffraction apparatus 200 according to Comparative Example 1. As shown in FIG. The X-ray diffraction apparatus 200 of Comparative Example 1 includes an X-ray source (not shown), a sample stage 230, a PSA 250, and a detector 260. For the basic configurations of the X-ray source, sample stage 230, and detector 260, please refer to the sample stage 130 and detector 160 of the first embodiment. The relationship between the diffraction angle 2θ and the goniometer angle 2Θ differs between the first embodiment and Comparative Example 1. Specifically, the detector 160 of the first embodiment converts a certain goniometer angle 2Θ into 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, the detector 260 of Comparative Example 1 treats a certain goniometer angle 2Θ as being equal to the diffraction angle 2θ.
[0042] The PSA 250 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 PSA 250's accuracy can be improved by narrowing the spacing between the foils and lengthening the optical path through the foils. However, if the spacing between the foils is shortened, the diffracted X-rays may be scattered by the foils. Detection of these scattered diffracted X-rays reduces accuracy. Measurements using the PSA 250 yield profiles with high accuracy but low intensity. Furthermore, even if the beam width of the diffracted X-rays widens, the resulting profile remains unchanged, enabling highly accurate measurements.
[0043] Comparative Example 2 FIG. 14 is a side view showing an example of an X-ray diffraction apparatus 300 according to Comparative Example 2. As shown in FIG. The X-ray diffraction apparatus 300 of Comparative Example 2 includes 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 the first embodiment.
[0044] Next, measurement results 1 to 5 will be described for the above-mentioned embodiment 1, comparative example 1, and comparative example 2.
[0045] [Measurement conditions] In the X-ray diffraction apparatus 100 of the first embodiment, the distance L between the goniometer center G and the front surface 150a of the slit member 150 S 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. The slit width W S is 0.15 mm. Strip width W D is 0.1 mm. In the X-ray diffraction apparatus 200 of Comparative Example 1, the aperture angle on the diagonal line between the foils arranged in parallel of the PSA 250 (the acute angle of the region between the two dashed lines in FIG. 13) is 0.114°. Furthermore, in the X-ray diffraction apparatus 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, a method for observing the profile obtained by X-ray diffraction measurement will be described. FIG. 15 is an example of a diagram illustrating the accuracy and precision in X-ray diffraction measurement. Peaks are observed in the profile obtained by X-ray diffraction measurement. The accuracy and precision of a sample can be determined by analyzing the position and intensity of these peaks. Accuracy is determined from the peak position. More specifically, accuracy is determined by the magnitude of the deviation between the reference position, which is the position where the peak should be obtained, and the actually measured peak position. That is, if the peak position is close to the reference position, the accuracy can be determined to be high. On the other hand, if the peak position is far from the reference position, the accuracy can be determined to be low. Accuracy is also determined from the peak width (more specifically, the full width at half maximum (FWHM)). More specifically, if the peak width is narrow, the accuracy can be determined to be high. On the other hand, if the peak width is wide, the accuracy can be determined to be low. Accuracy is also called angular accuracy.
[0047] [Measurement result 1: Strength comparison] FIG. 16 is a diagram showing an example of the results of measurements using the X-ray diffraction devices 100, 200, and 300. In Fig. 16, the solid line indicates the measurement results when the slit member 150 of embodiment 1 was provided. Also in Fig. 16, the dashed line indicates the measurement results when Comparative Example 1 was used, using PSA 250. Furthermore, in Fig. 16, the dashed line indicates the measurement results when Comparative Example 2 was used, using no slit or PSA. It can be seen that the X-ray diffraction apparatus 100 of embodiment 1 provides higher peak intensity and narrower peak width than the X-ray diffraction apparatus 200 of Comparative Example 1, which uses a PSA, and therefore is capable of high-intensity and high-precision measurements.
[0048] [Measurement result 2: Sample movement in the Z-axis direction] Next, the measurement results when the sample is moved in the vertical direction (Z-axis direction) will be described with reference to FIGS. Fig. 17 is a diagram showing an example of the results of measurement performed by moving sample F up and down using X-ray diffraction apparatus 100 in embodiment 1. Fig. 18 is a diagram showing an example of the results of measurement performed by moving sample F up and down using X-ray diffraction apparatus 200 in comparative example 1. Fig. 19 is a diagram showing an example of the results of measurement performed by moving sample F up and down using X-ray diffraction apparatus 300 in comparative example 2.
[0049] 17 to 19, the solid lines indicate the case where the sample F is placed at the goniometer center G. In addition, in Fig. 17 to 19, the dashed lines indicate the case where the sample F is moved upward by 0.5 mm from the goniometer center G. In addition, in Fig. 17 to 19, the dashed lines indicate the case where the sample F is moved downward by 0.5 mm from the goniometer center G.
[0050] 17, in Embodiment 1 using the slit member 150, no shift in peak position is observed even when the sample F is moved, and therefore accuracy is high. On the other hand, as shown in FIG. 18, in Comparative Example 1 using the PSA 250, no shift in peak position is observed when the sample F is moved, and therefore accuracy is high, but the accuracy is low compared to FIG. 17 because the peak shape cannot be observed accurately. Furthermore, as shown in FIG. 19, in Comparative Example 2 not using a slit or PSA, a shift in peak position is observed when the sample F is moved, and therefore accuracy is lacking. In variable temperature measurements, the sample position may change vertically depending on the temperature, and in such cases, this embodiment is found to be effective.
[0051] [Measurement result 3: Changing the tilt angle of the sample surface] Next, the results of measurements made by changing the tilt direction of the sample surface (rotating around the X axis) will be described with reference to FIGS. 20 to 22. Fig. 20 shows an example of the results of measurement performed by rotating the sample surface in the tilt direction using the X-ray diffraction apparatus 100 in embodiment 1. Fig. 21 shows an example of the results of measurement performed by rotating the sample surface in the tilt direction using the X-ray diffraction apparatus 200 in comparative example 1. Fig. 22 shows an example of the results of measurement performed by rotating the sample surface in the tilt direction using the X-ray diffraction apparatus 300 in comparative example 2.
[0052] 20 to 22, the solid lines indicate the case where the tilt angle of the sample F is 0° with respect to the goniometer center G. Also, in Fig. 20 to 22, the dashed lines indicate the case where the tilt angle of the sample F is 5° with respect to the goniometer center G.
[0053] 20 shows that in Embodiment 1, which uses the slit member 150, accurate peak shapes are observed and no shift in peak position is observed, resulting in high precision and accuracy, even when the sample surface is rotated in the tilt direction. On the other hand, FIG. 21 shows that in Comparative Example 1, which uses the PSA 250, no shift in peak position is observed when the sample surface is rotated in the tilt direction, resulting in high accuracy, but the peak shapes are not observed as accurately as in FIG. 20, resulting in low accuracy. Furthermore, FIG. 22 shows that in Comparative Example 2, which does not use a slit or PSA, no shift in peak position is observed when the sample surface is rotated in the tilt direction, resulting in high accuracy, but the peak width is broadened, resulting in low accuracy. Note that when a sample with an uneven surface is measured, the same effect as this measurement result occurs. Therefore, it is effective to use the slit member 150 even when measuring a sample with an uneven surface.
[0054] [Measurement result 4: Changing the beam width] Next, the results of measurements made by changing the beam width of the incident X-ray will be described with reference to FIGS. Fig. 23 is a diagram showing an example of measurement results when the beam width of the incident X-rays 120 is changed using the X-ray diffraction apparatus 100 in embodiment 1. Fig. 24 is a diagram showing an example of measurement results when the beam width of the incident X-rays 120 is changed using the X-ray diffraction apparatus 200 in comparative example 1. Fig. 25 is a diagram showing an example of measurement results when the beam width of the incident X-rays 120 is changed using the X-ray diffraction apparatus 300 in comparative example 2.
[0055] 23 to 25, the solid lines indicate the case where the incident beam width is 0.8 mm, the dashed lines indicate the case where the incident beam width is 0.4 mm, and the dashed lines indicate the case where the incident beam width is 0.1 mm.
[0056] 23, in the first embodiment using the slit member 150, even when the beam width of the incident X-rays is changed, no change in the peak shape is observed, and measurements can be made with high accuracy. On the other hand, in the first comparative example using the PSA 250, as shown in FIG. 24, when the beam width of the incident X-rays is changed, although an accurate peak shape cannot be observed compared to FIG. 23, no change in the peak shape is observed when the beam width of the incident X-rays is changed, and therefore the impact on accuracy is small. Furthermore, as shown in FIG. 25, in the second comparative example using neither a slit nor a PSA, when the beam width of the incident X-rays is changed, the peak width increases as the beam width of the incident X-rays increases, even though the peak has the same diffraction angle, and accuracy is reduced.
[0057] [Measurement result 5: Changing the incident angle of incident X-rays] The results of measurements taken by changing the incident angle of the incident X-ray onto the sample are explained below. Fig. 26 is a diagram showing an example of the results of measurements performed by changing the incident angle of incident X-rays 120 using the X-ray diffraction apparatus 100 in embodiment 1. Fig. 27 is a diagram showing an example of the results of measurements performed by changing the incident angle of incident X-rays 220 using the X-ray diffraction apparatus 200 in comparative example 1. Fig. 28 is a diagram showing an example of the results of measurements performed by changing the incident angle of incident X-rays using the X-ray diffraction apparatus 300 in comparative example 2.
[0058] 26 to 28, the solid lines show the results of measurements taken in a symmetrical arrangement (same incident angle and exit angle), while the dashed lines show measurements taken while fixing the incident angle at 1.0° and moving only the light-receiving side.
[0059] 26 shows that in embodiment 1, which uses slit member 150, no change in peak shape is observed when the incident angle of the incident X-rays is changed, and measurements can be made with high accuracy. On the other hand, as shown in FIG. 27, in comparative example 1, which uses PSA, no change in accuracy is observed when the incident angle of the incident X-rays is changed, but the peak shape is not observed as accurately as in FIG. 26, and accuracy is low. As shown in FIG. 28, in comparative example 2, which does not use a slit or PSA, when the incident angle of the incident X-rays is changed, the peak width increases, even though the peak has the same diffraction angle, and accuracy is reduced. When the incident angle is shallower than the outgoing angle, the beam width of the diffracted X-rays widens, resulting in the same state as when the beam width of the incident X-rays is widened in Measurement Result 4. In in-plane measurements or measurements of thin film materials, the incident angle relative to the sample surface is sometimes fixed at a small angle, and it is clear that this embodiment is effective in such cases.
[0060] From the above measurement results, it can be seen that embodiment 1 using slit member 150 can obtain high accuracy and high strength results compared to comparative example 1 using PSA 250. Furthermore, the effects on precision and accuracy caused by changes in the sample position, tilt angle of the sample surface, beam width of the incident X-rays, incident angle of the incident X-rays, etc., which were observed in comparative example 2 not using a slit or PSA, were not observed in embodiment 1.
[0061] [Variation 1] Fig. 29 is a side view showing an example of an X-ray diffraction apparatus 400 according to Modification 1 of Embodiment 1. Fig. 30 is a top view showing an example of an X-ray diffraction apparatus 400 according to Modification 1 of Embodiment 1. The X-ray diffraction apparatus 400 of the first modification includes 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, the sample stage 430, and the slit member 450, please refer to the sample stage 130 and the slit member 150 of the first embodiment.
[0062] The monochromator 470 has a grating surface that diffracts diffracted X-rays of a specific wavelength. The monochromator 470 is disposed between the slit member 450 and the detector 460 with the grating surface inclined in a direction from one end to the other in the longitudinal direction (B-axis direction) of the slit 451. The monochromator 470 is disposed in a direction perpendicular to the diffraction angle. The monochromator 470 monochromatizes the diffracted X-rays. In X-ray diffraction measurements using a powder sample, the monochromator 470 is mainly made of graphite, but is not limited to this.
[0063] Detector 460 is provided to detect diffracted X-rays of a specific wavelength diffracted by monochromator 470. That is, detector 460 is provided downstream of monochromator 470 with a detection surface 460a directed toward monochromator 470. Detector 460 is also provided shifted from monochromator 470 in the Y-axis direction.
[0064] Next, the case where the incident X-rays are non-parallel will be described with reference to FIGS. In particular, non-parallel incident X-rays 520, 620 can be applied when the traveling direction of the incident X-rays and the shape of the sample are known, except when the incident X-rays are focused on the sample.
[0065] [Variation 2] FIG. 31 is a side view showing an example of an X-ray diffraction apparatus 500 according to the second modification of the first embodiment. In the X-ray diffraction apparatus 500 of the second modification, an X-ray source (not shown) irradiates the sample F with incident X-rays 520 so that the X-rays 520 diverge in the direction of travel.
[0066] [Variation 3] FIG. 32 is a side view showing an example of an X-ray diffraction apparatus 600 according to the third modification of the first embodiment. In the X-ray diffraction apparatus 600 of the second modification, an X-ray source (not shown) irradiates the sample F with incident X-rays 620 so that the X-rays converge in the direction of travel.
[0067] [Variation 4] FIG. 33 is a side view showing an example of an X-ray diffraction apparatus 700 according to the fourth modification of the first embodiment. In the X-ray diffraction apparatus 700 of the fourth modification, a profile can be obtained while keeping the positions of the incident side of the X-ray source (not shown), the light receiving side of the detector 760, and the sample F on the sample stage 730 constant. In particular, it can be used when measuring changes over time using powder sample F, when measuring peak changes at short time intervals such as during temperature-controlled measurements, or when simply measuring a narrow range (one peak).
[0068] [Variation 5] FIG. 34 is a side view showing an example of an X-ray diffraction apparatus 800 according to the fifth modification of the first embodiment. The X-ray diffraction apparatus 800 of the fifth modification example includes an X-ray source (not shown), a sample stage 830, a slit member 850, a detector 860, and an interference prevention member 870. For the sample stage 830 and the detector 860, refer to the sample stage 130 and the detector 160 of the first embodiment.
[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 to each other.
[0070] The interference prevention member 870 is configured to prevent interference between the first diffracted X-ray 841 that passed through the first slit 851 and the second diffracted X-ray 842 that passed through the second slit 852 between the slit member 850 and the detector 860. That is, the interference prevention member 870 extends from the slit member 850 toward the detector 860. In other words, the interference prevention member 870 extends in the C-axis direction. The interference prevention member 870 may be made of stainless steel or the like as long as it has the property of blocking X-rays. The shape of the interference prevention member 870 is not limited to a plate shape as long as it is capable of blocking 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 supported on the slit member 850, the detector 860, or the arm of the goniometer.
[0071] In the fifth modification, the number of slits 851 and 852 is two, but any number can be selected to expand the detection area in the detector 860. Also, the number of interference prevention members 870 is one, but any number can be selected to prevent diffracted X-rays that have passed through different slits from interfering with each other.
[0072] Next, with reference to FIG. 35, a method of conversion to a diffraction angle 2θ when using X-ray diffraction apparatus 800 of Modification 5 will be described. In Modification 5 as well, the diffraction angle 2θ of diffracted X-rays 841 and 842 depends on the shortest distance L from the front surface 850a of slit member 850 to the detection surface 860a of detector 860. FIG. 35 is an enlarged view of the area surrounded by the dashed line in FIG. 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. Furthermore, the slit center lines SL1 and SL2 are straight lines that pass through the centers of the slits 851 and 852 in the short-side direction (A-axis direction) and extend in the B-axis direction. In variant 5, it is necessary to take into account the angle between the goniometer angle line AL and the line connecting 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) at the shortest distance, convert it into a diffraction angle 2θ, and then 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. Furthermore, 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 that passes through the first slit 851 and is detected at the X-ray detection position D=D1 is expressed by the following equation 4. Furthermore, the diffraction angle 2θ of the second diffracted X-ray 842 that passes through the second slit 852 and is detected at the X-ray detection position D=D2 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 direct measurement of diffraction from lattice planes perpendicular to the surface of the sample, thereby enabling direct evaluation of the structure near the surface, resulting in accurate evaluation of the sample.
[0077] FIG. 36 is a perspective view showing an example of an X-ray diffraction apparatus 900 according to the second embodiment. The X-ray diffraction apparatus 900 of the second embodiment includes an X-ray source (not shown), a sample stage 930, a slit member 950, and a detector 960. That is, the X-ray source irradiates incident X-rays 920, which are monochromatic and parallel to the surface of the sample, at a small angle of incidence. 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 grazing the sample surface. The 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] In the second embodiment, in order to detect the diffracted X-rays 940, the slit member 950 and the detector 960 are arranged so that the longitudinal directions of the slit 951 and the detection strip 961 are parallel to each other. Furthermore, in addition to the X-ray diffraction device 900 that performs in-plane measurement, an in-plane reciprocal lattice mapping device, a GI-WAXS / SAXS (Grazing-Incidence Wide-Angle X-Ray Scattering / Small-Angle X-Ray Scattering) device, or the like can also be used.
[0079] [others] The techniques disclosed in this specification can also be used for measurements using a pinhole and a two-dimensional detector. FIG. 37 is a perspective view showing an example of an X-ray diffraction apparatus 1000 that uses a pinhole member 1050 and a two-dimensional detector 1060. In the first and second embodiments, the cases where a slit and a one-dimensional detector are used have been described, but Debye rings can also be detected instead of a pinhole and a two-dimensional detector, respectively.
[0080] The X-ray diffraction apparatus 1000 of this embodiment includes 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 parallel incident X-rays 1020 toward the sample stage 1030. A pinhole 1051 is formed in the center of the pinhole member 1050 to allow diffracted X-rays to pass through. Of the X-rays diffracted by crystal lattice planes perpendicular to the sample surface, only diffracted X-rays 1040 that pass through the pinhole 1051 proceed toward the two-dimensional detector 1060. The two-dimensional detector 1060 detects the diffracted X-rays 1040 using pixels 1061, rather than a detection strip that extends in the width direction as in a one-dimensional detector. In yet 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 differ from one another, thereby replacing the pinhole member 1050. For example, a first slit member whose slit longitudinal direction extends in the A-axis direction and a second slit member whose slit 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 in this specification relates to an X-ray diffraction apparatus and measurement method that uses a slit (or pinhole) and a one-dimensional (or two-dimensional) detector, and the precision and accuracy of peaks are independent of the sample position and shape. Furthermore, data with higher intensity and precision can be obtained compared to measurements using PSA. Furthermore, the intensity and precision can be selected by changing the slit position, slit width, and the arrangement of the slit and detector.
[0082] It may be provided in the following manner. In the X-ray diffraction apparatus, the slit has a tapered shape so as to widen from the sample stage toward the detector. In the X-ray diffraction apparatus, the width of the slit in the short side direction is wider than the width of the detection strip in the short side direction. In the X-ray diffraction apparatus, the center of the goniometer circle, the center of the slit in the short direction, and the detection strip are arranged on a straight line. In the X-ray diffraction apparatus, the diffraction angle of the diffracted X-rays depends on the distance from the slit to the detector. An X-ray diffraction apparatus, wherein the distance between the slit and the detector depends on the diffraction angle of the diffracted X-rays, the angle of a goniometer and the distance from one detector strip to another. In the X-ray diffraction apparatus, the detector detects the diffracted X-rays with a first detection strip when a diffraction angle of the diffracted X-rays is equal to a goniometer angle, and detects the diffracted X-rays with a second detection strip when the diffraction angle is not equal to the goniometer angle. The X-ray diffraction apparatus further comprises an interference prevention member, the slit member having a first slit and a second slit, the longitudinal axis of the first slit and the longitudinal axis of the second slit being parallel, and the interference prevention member being configured to prevent interference between a first diffracted X-ray that has passed through the first slit and a second diffracted X-ray that has passed through the second slit, between the slit member and the detector. The X-ray diffraction apparatus further comprises a monochromator, the monochromator having a grating surface that diffracts the diffracted X-rays of a specific wavelength, and the grating surface is disposed between the slit member and the detector, with the grating surface being inclined in a direction from one end to the other end in the longitudinal direction of the slit. In the X-ray diffraction apparatus, the sample stage has a mounting surface on which the sample is placed and moves parallel to the mounting surface. In the X-ray diffraction apparatus, the sample stage has a mounting surface on which the sample is placed, and is configured to be rotatable about an axis so as to change the orientation of the mounting surface. In the X-ray diffraction apparatus, the X-rays irradiated from the X-ray source to the sample are parallel X-rays. A method for measuring a sample, comprising: irradiating the sample with X-rays, diffracting the X-rays, passing the diffracted X-rays through a slit, and detecting the diffracted X-rays one-dimensionally with a detection strip, thereby measuring the sample, wherein the longitudinal axis of the slit is parallel to the longitudinal axis of the detection strip. Of course, this is not the case.
[0083] Finally, while various embodiments according to the present disclosure have been described, these are presented as examples and are not intended to limit the scope of the invention. The novel embodiments may be embodied in various other forms, and various omissions, substitutions, and modifications may be made without departing from the spirit of the invention. The embodiments and modifications thereof are intended to be included within the scope and spirit of the invention, as well as within the scope of the inventions and their equivalents as defined in the claims. [Explanation of symbols]
[0084] 100: X-ray diffraction equipment 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 diffraction equipment 220: Incident X-ray 230: Sample stage 240: Diffraction X-rays 260: Detector 300: X-ray diffraction equipment 330: Sample stage 360: Detector 360a: detection surface 400: X-ray diffraction equipment 430: Sample stage 450: Slit member 451: Slit 460: Detector 460a: Detection surface 470: Monochromator 500: X-ray diffraction equipment 520: Incident X-ray 600: X-ray diffraction equipment 620: Incident X-ray 700: X-ray diffraction equipment 720: Incident X-ray 730: Sample stage 760: Detector 800: X-ray diffraction equipment 830: Sample stage 841: First diffracted X-ray 842: Second diffracted 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 diffraction equipment 920: Incident X-ray 930: Sample stage 940: Diffraction X-rays 950: Slit member 951: Slit 960: Detector 961:Detection strips 1000: X-ray diffractometer 1020: Incident X-ray 1030: Sample stage 1040: Diffraction X-rays 1050: Pinhole material 1051: Pinhole 1060: 2D detector 1061:pixels 2Θ: Goniometer angle 2θ: diffraction angle AL: Goniometer angle wire D: X-ray detection position DL: Detector center line F: Sample G: Center of goniometer GL: Goniometer center line L: distance L S :distance S: distance SL: Slit center line SL1: Slit center line SL2: Slit center line W D :Strip width W S :Slit width
Claims
1. An X-ray diffraction apparatus, The apparatus includes an X-ray source, a sample stage, a detector, and a slit member, the X-ray source is configured to be able to irradiate a sample with X-rays; the sample stage is configured so that the sample can be placed on it so that the X-rays are diffracted; the detector is configured to be able to detect diffracted X-rays, which are the diffracted X-rays, one-dimensionally using a detection strip; The slit member is provided between the sample stage and the detector, 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; X-ray diffraction equipment.
2. 2. The X-ray diffraction apparatus according to claim 1, the slit has a tapered shape so as to widen from the sample stage toward the detector; X-ray diffraction equipment.
3. 3. The X-ray diffraction apparatus according to claim 1, The width of the slit in the short side direction is wider than the width of the detection strip in the short side direction. X-ray diffraction equipment.
4. The X-ray diffraction apparatus according to any one of claims 1 to 3, the center of the goniometer circle, the center of the slit in the short direction, and the detection strip are arranged on a straight line; X-ray diffraction equipment.
5. 5. The X-ray diffraction apparatus according to claim 4, the diffraction angle of the diffracted X-rays depends on the distance from the slit to the detector; X-ray diffraction equipment.
6. 6. The X-ray diffraction apparatus according to claim 4 or claim 5, 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 detector strip to another. X-ray diffraction equipment.
7. The X-ray diffraction apparatus according to any one of claims 4 to 6, the detector detects the diffracted X-rays with a first detection strip when a diffraction angle of the diffracted X-rays is equal to a goniometer angle, and detects the diffracted X-rays with a second detection strip when the diffraction angle is not equal to the goniometer angle; X-ray diffraction equipment.
8. The X-ray diffraction apparatus according to any one of claims 1 to 7, An interference prevention member is provided, the slit member has a first slit and a second slit, a longitudinal axis of the first slit and a 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 slit member and the detector. X-ray diffraction equipment.
9. The X-ray diffraction apparatus according to any one of claims 1 to 8, Equipped with a monochromator, The monochromator is a grating surface that diffracts the diffracted X-rays of a specific wavelength, the grating surface is provided between the slit member and the detector, and is inclined in a direction from one end to the other end in the longitudinal direction of the slit; X-ray diffraction equipment.
10. The X-ray diffraction apparatus according to any one of claims 1 to 9, the sample stage has a mounting surface on which the sample is placed and moves parallel to the mounting surface; X-ray diffraction equipment.
11. The X-ray diffraction apparatus according to any one of claims 1 to 10, the sample stage has a mounting surface on which the sample is placed, and is configured to be rotatable about an axis so as to change the orientation of the mounting surface; X-ray diffraction equipment.
12. The X-ray diffraction apparatus according to any one of claims 1 to 11, The X-rays irradiated from the X-ray source to the sample are parallel X-rays. X-ray diffraction equipment.
13. A method for measuring a sample, comprising: irradiating the sample with X-rays and diffracting the X-rays; The diffracted X-rays are passed through a slit; measuring the sample by detecting the diffracted X-rays one-dimensionally with a detection strip; the longitudinal axis of the slit is parallel to the longitudinal axis of the detection strip; Measurement method.
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