JP2019184294A - X-ray analyzer and X-ray analysis method - Google Patents

Abstract

To provide an X-ray analyzer with which it is possible to easily analyze the crystal state in the thickness direction of a plate- or sheet-like sample.SOLUTION: The X-ray analyzer comprises: an X-ray source 10 for emitting an X-ray with which one surface of a plate- or sheet-like sample 100 is irradiated; a sample stage 20 on which the sample is installed; a first detector 30 for detecting a first diffraction X-ray having passed through the sample; and a second detector 40 for detecting a second diffraction X-ray having passed through the sample. The first detector is installed in the direction of a first angle 2θ1 relative to the normal of the other surface of the sample, and the second detector is installed in the direction of a second angle 2θ2 relative to the normal of the other surface of the sample, the first angle being smaller than the second angle.SELECTED DRAWING: Figure 1

Description

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

  The electrode material or the like forming the electrode of the dry battery is plate-shaped or sheet-shaped, and is formed of polycrystal having a crystal grain size of 1 to 100 μm. As a method for examining the crystal state of such an electrode, there are analysis by X-ray diffraction and microscopic observation using an electron microscope, an optical microscope, or the like.

JP-A-4-198745 JP 2005-528594 A Japanese Patent Laid-Open No. 9-281061

  Analysis by X-ray diffraction is a method in which X-rays are incident on a sample and the diffracted X-rays diffracted in the sample are measured. Generally, the measurement is performed by measuring the diffracted X-rays reflected from the sample. Is called. When considering the analysis of the crystal state in the thickness direction of the sample by such X-ray diffraction, it is necessary to change the X-ray source or adjust the irradiation energy. The analysis results may not be very accurate.

  Further, in the microscopic observation, it is necessary to destroy the electrode to be observed, and it takes time and labor to process it into a sample for observation. Further, since the resolution is not sufficient in microscopic observation, it is difficult to evaluate the crystal state such as the crystal structure.

  Therefore, there is a demand for an analyzer that can easily analyze the crystal state in the thickness direction of a plate-like or sheet-like sample to be analyzed.

  According to one aspect of the present embodiment, an X-ray source that emits X-rays irradiated on one surface of a plate-like or sheet-like sample, a sample stage on which the sample is installed, and the sample are transmitted A first detector for detecting the first diffracted X-ray, and a second detector for detecting the second diffracted X-ray transmitted through the sample, the first detector comprising: The second detector is installed in a second angular direction with respect to the normal direction of the other surface of the sample, and the second detector is installed in a second angular direction with respect to the normal direction of the other surface of the sample. The first angle is smaller than the second angle.

  According to the disclosed X-ray analyzer, it is possible to easily analyze the crystal state in the thickness direction of a plate-like or sheet-like sample.

Structure diagram of X-ray analyzer in the first embodiment Explanatory drawing of the X-ray analyzer in 1st Embodiment Flowchart of X-ray analysis method in the first embodiment Diffraction intensity characteristic diagram obtained by the X-ray analysis method in the first embodiment (1) Diffraction intensity characteristic diagram obtained by the X-ray analysis method in the first embodiment (2) Diffraction intensity characteristic diagram obtained by the X-ray analysis method in the first embodiment (3) Diffraction intensity characteristic diagram obtained by the X-ray analysis method in the first embodiment (4) Explanatory drawing of the analysis result of the sample obtained by the X-ray analysis method in the first embodiment Explanatory drawing of the analysis result of the other sample obtained by the X-ray-analysis method in 1st Embodiment Flowchart of a modified example of the X-ray analysis method in the first embodiment Structure diagram of X-ray analyzer in the second embodiment

  The form for implementing is demonstrated below. In addition, about the same member etc., the same code | symbol is attached | subjected and description is abbreviate | omitted.

[First Embodiment]
First, the analysis of the crystal state in the thickness direction of the sample was examined using an existing X-ray diffractometer. As a method of analyzing the crystal state in the thickness direction of a sample using existing X-ray diffraction, there are a method of changing the energy of X-rays incident on the sample and a method of changing the angle of X-rays incident on the sample. It is done.

  The method of changing the energy of X-rays incident on the sample utilizes the fact that changing the energy of X-rays incident on the sample changes the depth of X-rays that enter the material. In this method, every time the energy of X-rays incident on the sample is changed, it is necessary to change the setting of the X-ray diffractometer and readjustment, which cannot be easily performed. In X-ray diffractometers, the X-ray source often uses an X-ray tube or rotating anti-cathode that uses characteristic X-rays such as Cu, Co, Cr, and Mo. The range of possible X-ray energy choices is narrow.

  Next, the method of changing the angle of the X-rays incident on the sample utilizes the fact that when the X-rays are incident at a shallow angle with respect to the sample surface, the X-rays enter only a few nm from the surface of the sample. In this method, X-rays are made incident at a shallow angle with respect to the surface of the sample. In this case, it is easy to be affected by unevenness on the surface of the sample, and it is difficult to accurately control the incident angle of X-rays incident on the sample. Have difficulty. In addition, if a surface layer of a material different from the material to be analyzed exists on the surface of the sample, it becomes difficult to control the X-ray penetration length by changing the X-ray incident angle. This tendency is strong when the density of is higher than that of the material to be analyzed inside the sample. For this reason, in this method, it is not realistic to analyze the change in the crystal state of the material in the depth direction from the surface of the sample.

  Therefore, it is not easy to analyze a crystal state such as crystallinity, crystal structure, crystal phase, etc. in the thickness direction of a plate-like or sheet-like sample using an existing X-ray diffractometer.

(X-ray analyzer)
Next, the X-ray analyzer in the first embodiment will be described. The X-ray analyzer in the present embodiment includes an X-ray source 10, a sample stage 20, a first two-dimensional detector 30, a second two-dimensional detector 40, a control unit 50, a display unit 60, and the like. Yes.

  X-rays emitted from the X-ray source 10 are monochromatic X-rays. The sample stage 20 is for installing the sample 100 to be analyzed, and has rotation axes φ and ψ. The rotation axis ψ is an axis for changing the in-plane inclination of the sample 100, and the rotation axis φ is an axis for changing the plane on which the X-rays are incident. The sample 100 is placed on the sample stage 20 so that the sample surface is perpendicular to the X-rays incident on the sample 100 (incident X-rays).

The first two-dimensional detector 30 is a two-dimensional position-sensitive X-ray detector capable of detecting the incident position (x _j , y _j ) and intensity I _j of the first diffracted X-ray, It has a translation axis Xp for position adjustment that can move the first two-dimensional detector 30 in parallel with the X-ray incident surface.

The second two-dimensional detector 40 is a two-dimensional position-sensitive X-ray detector that can detect the incident position (x _k , y _k ) and intensity I _k of the second diffracted X-ray. The second two-dimensional detector 40 may also have a translation axis for position adjustment that can move the second two-dimensional detector 30 parallel to the X-ray incident surface.

The control unit 50 includes a position control unit 51, an X-ray measurement unit 52, an arithmetic processing unit 53, a storage unit 54, and the like, and is connected to a display unit 60 that can display a two-dimensional image or the like. The position control unit 51 is connected to the sample stage 20 and the first two-dimensional detector 30, controls the rotation axes φ and ψ in the sample stage 20, and translates in the first two-dimensional detector 30. Xp is controlled. The X-ray measurement unit 52 is connected to the first two-dimensional detector 30 and the second two-dimensional detector 40. The X-ray measurement unit 52 measures the incident position (x _j , y _j ) and intensity I _j of the X-ray detected by the first two-dimensional detector 30 and is detected by the second two-dimensional detector 40. The X-ray incident position (x _k , y _k ) and intensity I _k are measured. The arithmetic processing unit 53 calculates a histogram from the measured X-ray incident position and intensity, calculates an X-ray diffraction profile indicating the relationship between the diffraction angle and the diffraction intensity, and calculates a lattice constant. I do. The storage unit 54 stores information such as the result calculated by the arithmetic processing unit 53. The display unit 60 can display various types of information including information about the X-ray spot detected by the first two-dimensional detector 30 and the second two-dimensional detector 40.

In the present embodiment, the first two-dimensional detector 30 is in the first angle (2θ ₁ ) direction with respect to the normal direction of the other surface 100b of the sample 100 from which the X-ray incident on the sample 100 is emitted. The second two-dimensional detector 40 is arranged in the _second angle (2θ ₂ ) direction. Note that θ ₁ <θ ₂ , the first angle (2θ ₁ ) is greater than 0 ° and less than 60 °, and the second angle (2θ ₂ ) is in the range of 60 ° to 90 °.

  More specifically, as shown in FIG. 2, in the X-ray analysis apparatus according to the present embodiment, the monochromatic X-ray emitted from the X-ray source 10 becomes an incident X-ray and becomes the sample surface of the sample 100. Is incident perpendicular to the surface 100a. Thus, the incident X-ray incident on the sample 100 is diffracted in the sample 100 and emitted from the other surface 100 b of the sample 100. The diffracted X-rays emitted from the other surface 100b of the sample 100 include a first diffracted X-ray and a first diffracted X-ray that are diffracted at a narrow angle with respect to the normal direction of the other surface 100b of the sample 100. There is a second diffracted X-ray that is diffracted at a wider angle.

  The first diffracted X-ray is diffracted in the thickness direction of the sample 100, that is, in each region between the one surface 100a and the other surface 100b of the sample 100. The crystal state information is reflected. Thus, the first diffracted X-rays emitted from the other surface 100b of the sample 100 are arranged in a narrow angle direction with respect to the normal direction of the other surface 100b of the sample 100. Is detected. Note that the X-rays incident on the inside of the sample 100 are absorbed inside the sample 100, but the diffracted X-rays diffracted near the one surface 100a of the sample 100 are also near the other surface 100b of the sample 100. The distance that the diffracted X-rays diffracted through the sample 100 pass through the sample 100 is substantially the same. Therefore, X-rays transmitted through the sample 100 have the same X-ray dose absorbed in the sample 100, and uniform crystal state information in the thickness direction of the sample 100 can be obtained.

  On the other hand, the second diffraction X-ray is diffracted at a wide angle with respect to the normal direction of the other surface 100b of the sample 100, that is, at a shallow angle with respect to the other surface 100b. For this reason, the diffracted X-ray diffracted in the region deeper than the other surface 100b of the sample 100 has a longer distance to travel inside the sample 100, and therefore is absorbed exponentially inside the sample 100. Almost never appears. On the other hand, the diffracted X-ray diffracted in the shallow region near the other surface 100b of the sample 100 has a short distance to travel through the sample 100, and therefore has little absorption in the sample 100, and the other surface of the sample 100. 100b is emitted as the second diffracted X-ray. In this way, the second diffracted X-ray emitted from the other surface 100b of the sample 100 is the second two-dimensional detector 40 arranged in a wide angle direction with respect to the normal direction of the other surface 100b of the sample 100. Is detected.

  Therefore, in the X-ray analyzer according to the present embodiment, the entire crystal state in the thickness direction of the sample 100 and information on the crystal state of the shallow region near the other surface 100b of the sample 100 are simultaneously acquired. Can do. Thereby, it is possible to easily know what the crystalline state of the shallow region in the vicinity of the other surface 100b of the sample 100 is as compared with the entire crystalline state in the thickness direction of the sample 100. it can.

Note that the X-ray analyzer in the present embodiment measures and analyzes the diffracted X-rays transmitted through the sample 100. For this reason, when the thickness of the sample 100 is thick, the X-rays incident on the sample 100 are absorbed inside the sample 100 and the sample 100 cannot be analyzed. Therefore, the sample 100 to be measured in the X-ray analyzer according to the present embodiment is a plate-like or sheet-like sample. Specifically, when CuK rays are used as the X-ray source 10, if the density of the material forming the sample 100 is 4 g / cm ³ , the thickness of the sample 100 can be up to 500 μm. Further, when a high energy X-ray such as a MoK ray is used as the X-ray source 10, the sample 100 can handle a thickness of up to 5 mm. In addition, although the thickness of the sample 100 which can respond | corresponds depends on the density of the material which forms the sample 100, in this Embodiment, it is preferable that the thickness of the sample 100 is 5 mm or less.

(X-ray analysis method)
Next, the X-ray analysis method in the present embodiment will be described based on the flowchart shown in FIG. The X-ray analysis method in the present embodiment is performed using the X-ray analysis apparatus in the present embodiment shown in FIG. 1, and the case where the sample 100 is an Al plate having a thickness of 0.2 mm will be described. .

  First, as shown in step 102 (S102), the sample 100 is set on the sample stage 20, and monochromatic X-rays having a wavelength of 1.16 nm are emitted from the X-ray source 10 and irradiated toward the sample 100. The sample 100 is placed on the sample stage 20 so that monochromatic X-rays irradiated from the X-ray source 10 are incident on the one surface 100a of the sample 100 substantially perpendicularly. Thus, the incident X-rays incident on the sample 100 are diffracted in the sample 100, pass through the sample 100, and are emitted from the other surface 100b of the sample 100 as diffracted X-rays. Thus, among the diffracted X-rays emitted from the other surface 100b, 111 diffracted X-rays diffracted at an angle close to the traveling direction of the incident X-rays become the first diffracted X-ray, and the other surface 100b of the sample 100 422 diffracted X-rays diffracted at an angle nearly parallel to the second diffracted X-ray. Note that the 422 diffraction X-ray serving as the second diffraction X-ray has an angle of 0.2 ° with respect to the other surface 100b of the sample 100, that is, 89.8 with respect to the normal direction of the other surface 100b of the sample 100. X-ray diffraction diffracted at °. Therefore, the information on the crystal state in the region having a depth of 20 μm from the other surface 100b of the sample 100 is reflected.

  Next, as shown in step 104 (S104), the first two-dimensional detector 30 detects the first diffracted X-ray of the sample 100, and the first diffracted X-ray as shown in FIG. The relationship between 2θ and the diffraction intensity distribution is obtained. In the present application, this process may be referred to as a first detection process.

  Next, as shown in step 106 (S106), the second two-dimensional detector 40 detects the second diffracted X-ray of the sample 100, and the second diffracted X-ray as shown in FIG. The relationship between 2θ and the diffraction intensity distribution is obtained. In the present application, this step may be referred to as a second detection step. Note that the X-ray diffraction intensity in FIG. 5 is normalized by the peak intensity of 111 diffraction X-rays shown in FIG.

Next, as shown in step 108 (S108), the arithmetic processing unit 53 calculates Δ1 / d and the intensity distribution from the diffraction intensity distribution of the first diffracted X-ray detected by the first two-dimensional detector 30. Get a relationship. Specifically, from the diffraction intensity distribution of the first diffracted X-ray detected by the first two-dimensional detector 30 obtained in step 104, the peak of 111 diffracted X-rays that are the first diffracted X-rays. The value of 2θ that becomes the strength is obtained. Then, the value of 1 / d _p of 2θ that becomes the peak intensity is calculated from 2d _p sin θ = λ. That is, the value of 1 / d _p corresponding to 2θ, which is the peak intensity of 111 diffraction X-rays, is 28.726 °. Thereafter, 2θ in FIG. 4 is converted to 1 / d from 2dsinθ = λ, Δ1 / d is calculated from Δ1 / d = (1 / d) − (1 / d _p ), and the calculated Δ1 / d is calculated. Is the horizontal axis and the diffraction intensity is the vertical axis, a diffraction intensity distribution of the first diffraction X-ray as shown in FIG. 6 is obtained. In the diffraction intensity distribution of 111 diffracted X-rays thus obtained, the position of the peak of 111 diffracted X-ray is a position where Δ1 / d is 0. The wavelength λ is the wavelength of monochromatic X-rays emitted from the X-ray source 10.

Next, as shown in step 110 (S110), the arithmetic processing unit 53 calculates Δ1 / d and the intensity distribution from the diffraction intensity distribution of the second diffracted X-ray detected by the second two-dimensional detector 40. Get a relationship. Specifically, first, a lattice constant of 4.0497Å is calculated based on the value of 2θ that is the peak intensity of 111 diffraction X-rays as the first diffracted X-ray, and 1 / d is calculated from the lattice constant of 4.0497Å. Calculate the value of _p . Thereafter, 2θ in FIG. 5 is converted to 1 / d from 2dsinθ = λ, Δ1 / d is calculated from Δ1 / d = (1 / d) − (1 / d _p ), and the calculated Δ1 / d is calculated. With the horizontal axis as the horizontal axis and the vertical axis as the diffraction intensity, a diffraction intensity distribution of the second diffraction X-ray as shown in FIG. 7 is obtained. In the diffraction intensity distribution of 422 diffraction X-rays obtained in this way, the position where Δ1 / d is 0 is the position of the peak of 422 diffraction X-rays assumed when the peak of 111 diffraction X-rays is used as a reference. .

  FIG. 8 shows a combination of the results obtained in FIG. 6 and the results obtained in FIG. As shown in FIG. 8, the peak of the 422 diffraction X-ray, which is the second diffraction X-ray, is about −0. 003 is off. This shift means a shift in the lattice constant, which means that about 0.26% of the crystal state of the entire sample 100 is expanded in the region of the other surface 100b of the sample 100 up to a depth of 20 nm. means. Therefore, it can be seen that the sample 100 expands by 0.2 to 0.3% with respect to the entire crystal state of the sample 100 in the region from the other surface 100b to a depth of 20 nm.

  In the above description, the case where the lattice constant is calculated using the peak of 111 diffraction X-rays which is the first diffraction X-ray has been described. However, when analyzing a sample having a crystal structure with low symmetry, the first is used. The lattice constant may be calculated using a plurality of peaks detected by the two-dimensional detector 30. If the material forming the sample 100 is specified, the value of the lattice constant described in the literature may be used.

  FIG. 9 shows the results of analysis by the same X-ray analysis method as described above using another Al plate having a thickness of 0.2 mm as a sample. As shown in FIG. 9, in this sample, the shift of Δ1 / d of the peak of the 422 diffraction X-ray that is the second diffraction X-ray is different from the peak of the 111 diffraction X-ray that is the first diffraction X-ray. 0.001 or less. Therefore, it can be seen that the expansion of the region from the other surface of the sample to 20 nm with respect to the entire sample is not so large.

  Further, as shown in FIG. 9, this sample has a peak of the 422 diffraction X-ray that is the second diffraction X-ray with respect to the full width at half maximum W1 of the peak of the 111 diffraction X-ray that is the first diffraction X-ray. The full width at half maximum W2 is increased. Therefore, there is a difference between the average size of crystal grains in the entire thickness direction of the sample and the size of crystal grains in a region at 20 nm in the depth direction from the other surface of the sample. Specifically, it can be seen that the average crystal grain size in the region of 20 nm in the depth direction from the other surface of the sample is smaller than the average crystal grain size in the entire thickness direction of the sample.

  As described above, in the X-ray analysis method according to the present embodiment, the difference between the average in the thickness direction of the sample and the vicinity of the other surface of the sample is easy with respect to the crystal state such as the lattice constant and the crystal grain size. Can know.

  In the present embodiment, the one surface 100a and the other surface 100b of the sample 100 can be reversed by rotating the rotation axis φ of the sample stage 20 by 180 °. Thereby, monochromatic X-rays are incident from the other surface 100b of the sample 100, and the crystal state of the region in the vicinity of the one surface 100a of the sample 100 can be known.

  Specifically, based on FIG. 10, the crystal state on both surfaces of the sample 100, that is, both the crystal state in the region near one surface 100a of the sample 100 and the crystal state in the region near the other surface 100b are analyzed. The case where it does is demonstrated.

  First, as shown in step 202 (S202), monochromatic X-rays are made incident from one surface 100a of the sample 100, and the same analysis as in FIG. 3 is performed. Specifically, the first two-dimensional detector 30 detects the first diffracted X-ray of the sample 100 (first detection step), and the second two-dimensional detector 40 detects the second of the sample 100. Diffraction X-ray detection (second detection step) is performed. Thereby, information on the entire crystal state in the thickness direction of the sample 100 and the crystal state of the region in the vicinity of the other surface 100b of the sample 100 can be obtained.

  Next, as shown in step 204 (S204), the rotation axis φ of the sample stage 20 is rotated by 180 ° so that the one surface 100a and the other surface 100b of the sample 100 are reversed.

  Next, as shown in step 206 (S206), monochromatic X-rays are made incident from the other surface 100b of the sample 100, and the same analysis as in FIG. 3 is performed. Specifically, the first two-dimensional detector 30 detects the first diffracted X-ray of the sample 100 (third detection step), and the second two-dimensional detector 40 detects the second of the sample 100. Diffraction X-ray detection (fourth detection step) is performed. Thereby, information on the entire crystal state in the thickness direction of the sample 100 and the crystal state of the region in the vicinity of the one surface 100a of the sample 100 can be obtained.

  Through the above steps, the crystal state of both surfaces of the sample 100, that is, the crystal state of the region near the one surface 100a of the sample 100 and the crystal state of the region near the other surface 100b can be known.

[Second Embodiment]
Next, an X-ray analyzer according to the second embodiment will be described. The X-ray analyzer in the present embodiment is an X-ray analyzer having a structure in which three or more two-dimensional detectors capable of detecting diffracted X-rays diffracted at different angles are provided. FIG. 11 shows an X-ray analysis apparatus according to the present embodiment having a structure in which three two-dimensional detectors capable of detecting diffracted X-rays diffracted at different angles are provided.

Specifically, the X-ray analysis apparatus in the present embodiment includes an X-ray source 10, a sample stage 20, a first two-dimensional detector 30, a second two-dimensional detector 40, and a third two-dimensional detector. 170, a control unit 50, a display unit 60, and the like. In the present embodiment, the third two-dimensional detector 170 is arranged in the _third angle (2θ ₃ ) direction with respect to the normal direction of the other surface 100 b of the sample 100.

The third two-dimensional detector 170, a third incident position (x _{m, y m)} of the diffracted X-ray intensity I _m capable of detecting the two-dimensional type position-sensitive X-ray detector. The first two-dimensional detector 30 is arranged in the _first angle (2θ ₁ ) direction with respect to the normal direction of the other surface 100b of the sample 100 in order to detect the first diffracted X-ray. The two two-dimensional detector 40 is arranged in the _second angle (2θ ₂ ) direction in order to detect the first diffracted X-ray. Note that θ ₁ <θ ₃ <θ ₂ .

  By increasing the number of two-dimensional detectors in this way, the crystal state in the film thickness direction of the sample can be known in more detail and accurately.

  The contents other than the above are the same as in the first embodiment.

  Although the embodiment has been described in detail above, it is not limited to the specific embodiment, and various modifications and changes can be made within the scope described in the claims.

In addition to the above description, the following additional notes are disclosed.
(Appendix 1)
An X-ray source that emits X-rays applied to one surface of a plate-like or sheet-like sample;
A sample stage on which the sample is installed;
A first detector for detecting first diffracted X-rays transmitted through the sample;
A second detector for detecting second diffracted X-rays transmitted through the sample;
Have
The first detector is disposed in a first angular direction with respect to a normal direction of the other surface of the sample;
The second detector is installed in a second angular direction with respect to the normal direction of the other surface of the sample,
An X-ray analyzer characterized in that the first angle is smaller than the second angle.
(Appendix 2)
Having a control unit,
The control unit calculates a lattice constant of the sample based on the peak of the first diffracted X-ray detected by the first detector, and the second diffracted X detected by the second detector. The X-ray analyzer according to appendix 1, wherein a relationship between a deviation from the lattice constant at the peak of the line and a diffraction intensity is calculated.
(Appendix 3)
A third detector for detecting a third diffracted X-ray transmitted through the sample;
The third detector is installed in a third angular direction with respect to the normal direction of the other surface of the sample,
The X-ray analyzer according to Supplementary Note 1 or 2, wherein the first angle <the third angle <the second angle.
(Appendix 4)
Irradiating one surface of the sample with X-rays;
A first detection step of detecting a first diffracted X-ray transmitted through the sample by a first detector;
A second detection step of detecting a second diffracted X-ray transmitted through the sample by a second detector;
Have
The first detector is disposed in a first angular direction with respect to a normal direction of the other surface of the sample;
The second detector is installed in a second angular direction with respect to the normal direction of the other surface of the sample,
An X-ray analysis method, wherein the first angle is smaller than the second angle.
(Appendix 5)
Based on the peak of the first diffracted X-ray detected by the first detector, the lattice constant of the sample is calculated, and the peak of the second diffracted X-ray detected by the second detector is calculated. The X-ray analysis method according to appendix 4, characterized by comprising a step of calculating the relationship between the deviation from the lattice constant and the diffraction intensity.
(Appendix 6)
After the second detection step, rotating the sample 180 °;
Irradiating the other surface of the sample with X-rays;
A third detection step of detecting the first diffracted X-ray transmitted through the sample by a first detector;
A fourth detection step of detecting a second diffracted X-ray transmitted through the sample by a second detector;
The X-ray analysis method according to appendix 4 or 5, characterized by comprising:

10 X-ray source 20 Sample stage 30 First two-dimensional detector 40 Second two-dimensional detector 50 Control unit 51 Position control unit 52 X-ray measurement unit 53 Arithmetic processing unit 54 Storage unit 60 Display unit 100 Sample

Claims (6)

An X-ray source that emits X-rays applied to one surface of a plate-like or sheet-like sample;
A sample stage on which the sample is installed;
A first detector for detecting first diffracted X-rays transmitted through the sample;
A second detector for detecting second diffracted X-rays transmitted through the sample;
Have
The first detector is disposed in a first angular direction with respect to a normal direction of the other surface of the sample;
The second detector is installed in a second angular direction with respect to the normal direction of the other surface of the sample,
An X-ray analyzer characterized in that the first angle is smaller than the second angle. Having a control unit,
The control unit calculates a lattice constant of the sample based on the peak of the first diffracted X-ray detected by the first detector, and the second diffracted X detected by the second detector. The X-ray analyzer according to claim 1, wherein a relationship between a deviation from the lattice constant at a peak of the line and a diffraction intensity is calculated. A third detector for detecting a third diffracted X-ray transmitted through the sample;
The third detector is installed in a third angular direction with respect to the normal direction of the other surface of the sample,
3. The X-ray analyzer according to claim 1, wherein the first angle <the third angle <the second angle. Irradiating one surface of the sample with X-rays;
A first detection step of detecting a first diffracted X-ray transmitted through the sample by a first detector;
A second detection step of detecting a second diffracted X-ray transmitted through the sample by a second detector;
Have
The first detector is disposed in a first angular direction with respect to a normal direction of the other surface of the sample;
The second detector is installed in a second angular direction with respect to the normal direction of the other surface of the sample,
An X-ray analysis method, wherein the first angle is smaller than the second angle.   Based on the peak of the first diffracted X-ray detected by the first detector, the lattice constant of the sample is calculated, and the peak of the second diffracted X-ray detected by the second detector is calculated. The X-ray analysis method according to claim 4, further comprising a step of calculating a relationship between the deviation from the lattice constant and the diffraction intensity. After the second detection step, rotating the sample 180 °;
Irradiating the other surface of the sample with X-rays;
A third detection step of detecting a first diffracted X-ray transmitted through the sample by a first detector;
A fourth detection step of detecting a second diffracted X-ray transmitted through the sample by a second detector;
The X-ray analysis method according to claim 4 or 5, wherein:

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