JP3626965B2 - X-ray apparatus and X-ray measurement method - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to an X-ray apparatus and an X-ray measurement method for measuring a crystal structure and the like of a sample using X-rays.
[0002]
[Prior art]
In an apparatus for measuring the internal state of a sample using X-rays in a nondestructive manner, that is, an X-ray apparatus, it is necessary to place a sample to be measured at a predetermined position. In order to meet this need, conventionally, a method is known in which a sample plate is placed in a predetermined position with respect to the X-ray optical path while the sample is loaded on the sample plate.
[0003]
Conventionally, a glass sample plate formed of glass is known as such a sample plate. However, when measurement is performed with a small amount of sample supported by this glass sample plate, the X-rays directed to the sample enter the glass sample plate because of the small amount of the sample, and the glass halo (non- The background increases due to (crystallite scattering), and therefore the P / B ratio (that is, the Peak / Background ratio) decreases and the measurement accuracy decreases.
[0004]
As a conventional sample plate, a so-called single crystal sample plate formed of a single crystal such as Si (silicon) is also known. This single crystal sample plate is formed of a single crystal material having a crystal lattice plane that does not diffract X-rays incident on the sample. If this is used, the amount of the sample is so small that X-rays are single crystals. Even when it is incident on the sample plate, it is possible to prevent diffraction X-rays from being emitted from the single crystal sample plate, and as a result, a high P / B ratio can be obtained.
[0005]
Conventionally, a micro X-ray diffraction apparatus as shown in FIG. 7 is known. In this X-ray diffractometer, the sample S is rotated in a state where the incident angle of the incident X-ray R0 incident on the minute sample S is set to a predetermined value by rotating the minute sample S around the ω axis by the ω rotating device 53. Is rotated around the χ axis by the χ (chi) rotating device 51, and further rotated around the φ axis by the φ rotating device 56, that is, in-plane. Then, a diffracted X-ray R1 generated from the sample S is detected by a PSPC (Position Sensitive Proportional Counter) 57 as a one-dimensional detector.
[0006]
The reason why the sample S is rotated in the χ-axis and φ-axis in this way is that, since the number of crystals contained in the micro sample S is small, the X-ray diffraction measurement is performed while the sample S is kept stationary. In such a case, the sample S can be obtained by rotating the sample S around two orthogonal axes of the χ axis rotation and the φ axis rotation. This is because it is necessary to move randomly with respect to the X-rays.
[0007]
Randomly moving the sample S by orthogonal two-axis rotation is not limited to the micro X-ray diffractometer, and may be necessary for various X-ray diffraction measurements. When a plate is used, it is necessary to rotate the single crystal sample plate in the same biaxial direction in order to rotate the sample S in two orthogonal axes. At that time, the crystal lattice plane of the single crystal sample plate is relative to the incident X-ray. A state that satisfies the diffraction conditions appears, and a diffracted X-ray from the sample S that is the measurement target is generated from the single crystal sample plate separately from the sample S that is the measurement target. There is a risk that accurate measurement will not be possible due to the overlap.
[0008]
[Problems to be solved by the invention]
The present invention has been made in view of the above-described conventional problems, and eliminates the influence of diffracted X-rays from a sample plate supporting a sample, and performs very accurate X-ray diffraction measurement on the sample. An object of the present invention is to provide an X-ray apparatus and an X-ray measurement method capable of performing the above.
[0009]
[Means for Solving the Problems]
(1) In order to achieve the above object, an X-ray apparatus according to the present invention includes an X-ray exposure unit that irradiates a sample with X-rays and detects diffracted X-rays generated from the sample, and the X-ray exposure unit An X-ray apparatus having an X-ray reading unit for reading the diffracted X-rays detected in (1). The X-ray exposure unit is disposed around the sample plate, a single crystal sample plate that is formed of a single crystal substance and supports the sample, an X-ray source that emits X-rays toward the sample, and the like. A two-dimensional X-ray detector. The X-ray reading unit reads the data in the two-dimensional X-ray detector in a plane and outputs it as a signal, and based on the output signal of the X-ray reading means Integrating X-ray intensities belonging to the same diffraction angle Calculation means for obtaining diffraction X-ray intensity distribution by calculation When, A coordinate position at which the diffracted X-rays emitted from the single crystal sample plate are detected by the two-dimensional X-ray detector. Storage means for storing. And The computing means is The coordinate position of the diffracted X-ray from the single crystal sample plate stored by the storage means is excluded from the integration target. It is characterized by that.
[0010]
According to this X-ray apparatus, the diffracted X-ray generated from the single crystal sample plate is recognized as a blank region and excluded from the calculation. Therefore, when performing X-ray measurement on the sample supported by the single crystal sample plate, By eliminating the influence of diffracted X-rays from the single crystal sample plate, it is possible to perform very accurate X-ray diffraction measurement on the sample.
[0011]
As the X-ray detector, a so-called zero-dimensional X-ray detector having a structure for capturing X-rays in a dot shape, such as PC (Proportional Counter), SC (Scintillation Counter), PSPC, There is a so-called one-dimensional X-ray detector or the like having a structure for capturing X-rays in a straight line. The two-dimensional X-ray detector in the above configuration is an X-ray detector that can detect an X-ray at an arbitrary point in a plane, unlike the zero-dimensional X-ray detector or the one-dimensional X-ray detector. is there. As such a two-dimensional X-ray detector, for example, an X-ray film, a photostimulable phosphor or the like can be considered.
[0012]
The “blank area” is an area that does not contribute to the calculation of the diffracted X-ray intensity distribution, and various specific processes for realizing this area can be considered. For example, in a normal calculation, the calculation of integrating intensity data within the same diffraction angle (2θ) portion in a two-dimensional X-ray detector is often performed. In that case, the coordinate position corresponding to the blank area is set. A method of inserting “0” as data is conceivable.
[0013]
(2) Regarding the X-ray apparatus having the above-described configuration, φ rotation means for rotating the sample in the plane can be provided. In this way, even when the sample is very small, the diffracted X-rays generated from the sample can be captured at any timing during in-plane rotation.
[0014]
(3) Regarding the X-ray apparatus having the above-described configuration, the tilt moving means for tilting and moving the sample surface of the sample with respect to the two-dimensional X-ray detector, and the sample for changing the X-ray incident angle with respect to the sample And a ω rotation means for rotating the. If the tilt moving means is provided, the angular position of the sample with respect to the two-dimensional X-ray detector can be adjusted to an appropriate position, and if the ω rotation means is further provided, the incident angle of incident X-rays to the sample can be adjusted to an appropriate position.
[0015]
(4) In the X-ray apparatus configured as described above, the two-dimensional X-ray detector is preferably formed of a stimulable phosphor. This stimulable phosphor is an energy storage type radioactive detector, and is a stimulable phosphor, such as BaFBr: Er. ²⁺ Is formed on the surface of a flexible film, a flat film, or another member by coating or the like. This photostimulable phosphor is an object that can accumulate X-rays and the like in the form of energy, and can emit the energy as light to the outside by irradiation of stimulating excitation light such as laser light.
[0016]
That is, when the photostimulable phosphor is irradiated with X-rays or the like, energy is accumulated as a latent image inside the photostimulable phosphor corresponding to the irradiated portion, and further, laser light or the like is stored in the photostimulable phosphor. When the excitation light such as the above is irradiated, the latent image energy is emitted to the outside as light. By detecting the emitted light with a phototube or the like, the diffraction angle and intensity of X-rays that contributed to the formation of the latent image can be measured. This photostimulable phosphor has a sensitivity 10 to 60 times that of a conventional X-ray film. ⁵ -10 ⁶ With a wide dynamic range.
[0017]
(5) In the X-ray apparatus having the above-described configuration, it is desirable that the sample surface of the sample be inclined by 45 ° with respect to the central axis of the two-dimensional X-ray detector. By doing so, both the diffracted X-rays emitted from the sample along the sample surface tangential direction and the diffracted X-rays emitted along the sample surface vertical direction can be reliably detected by the two-dimensional X-ray detector. That is, it is possible to widen the diffracted X-ray capturing range by the two-dimensional X-ray detector.
[0018]
(6) Next, in the X-ray measurement method according to the present invention, a sample is supported by a single crystal sample plate formed of a single crystal substance, the sample is irradiated with X-rays, and diffracted X-rays generated from the sample Is detected by a two-dimensional X-ray detector disposed around the sample, the coordinates and intensity of the diffracted X-ray detected by the two-dimensional X-ray detector are read by the X-ray reading means, and the X-ray reading is performed. Based on the output signal of the means Integrating X-ray intensities belonging to the same diffraction angle An X-ray measurement method for obtaining a diffracted X-ray intensity distribution by calculation by a calculation means, wherein a coordinate position where a diffracted X-ray emitted from the single crystal sample plate is detected by the two-dimensional X-ray detector is determined. Store in the storage means before the calculation by the calculation means, The computing means is During the calculation by the calculation means, the coordinate position of the diffracted X-ray from the single crystal sample plate stored by the storage means is excluded from the integration target. It is characterized by that.
[0019]
According to this X-ray measurement method, the diffracted X-ray generated from the single crystal sample plate is recognized as a blank region and excluded from the calculation. Therefore, when performing X-ray measurement on the sample supported by the single crystal sample plate, The influence of the diffracted X-ray from the single crystal sample plate can be eliminated, and a very accurate X-ray diffraction measurement can be performed on the sample.
[0020]
(7) In the X-ray measurement method having the above-described configuration, the single crystal sample plate in a state in which the sample is not supported is irradiated with X-rays, and diffracted X-rays from the single crystal sample plate are detected by the two-dimensional X-ray detector. Then, the coordinate position of the diffracted X-ray obtained at that time can be set as the blank region, and then the sample can be supported by the single crystal sample plate for measurement.
[0021]
(8) Moreover, in the X-ray measuring method of the said structure, it can measure while rotating the said sample in plane. In this way, even when the sample is very small, the diffracted X-rays generated from the sample can be captured at any timing during in-plane rotation.
[0022]
(9) In the X-ray measurement method having the above-described configuration, the two-dimensional X-ray detector can be formed of a stimulable phosphor. In this way, it is possible to perform measurement with higher accuracy than when an X-ray film or the like is used.
[0023]
(10) In the X-ray measurement method having the above-described configuration, it is desirable that the sample surface of the sample be measured in a state inclined by 45 ° with respect to the central axis of the two-dimensional X-ray detector. By doing so, both the diffracted X-rays emitted from the sample along the sample surface tangential direction and the diffracted X-rays emitted along the sample surface vertical direction can be reliably detected by the two-dimensional X-ray detector. That is, it is possible to widen the diffracted X-ray capturing range by the two-dimensional X-ray detector.
[0024]
DETAILED DESCRIPTION OF THE INVENTION
1 and 3 show an embodiment of an X-ray apparatus when the present invention is applied to a micro X-ray diffraction apparatus. This micro X-ray diffraction apparatus is constituted by an X-ray exposure unit R shown in FIG. 1 and an X-ray reading unit T shown in FIG.
[0025]
The X-ray exposure unit R includes an X-ray source that emits X-rays, that is, an X-ray focal point F, a monochromator 3 that monochromaticizes X-rays emitted from the X-ray focal point F, and an X-ray that is monochromatic by the monochromator 3. A collimator 4 for extracting a line as a parallel X-ray beam having a small cross-sectional diameter, a sample support device 1 for supporting the sample S, and a two-dimensional X-ray detector arranged in a cylindrical shape around the sample S A fluorescent phosphor 2.
[0026]
The X-ray focal point F is formed, for example, as a point-focused X-ray focal point. Further, the monochromator 3 is constituted by, for example, a flat graphite crystal. The collimator 4 forms a parallel X-ray beam having a cross-sectional diameter of 10 to 100 μm, for example. The inner surface of the photostimulable phosphor 2 is a phosphor screen.
[0027]
The sample support device 1 includes a φ rotation device 6 that rotates the sample S around the φ axis, that is, an in-plane rotation, an arc swing mechanism 7 that rotates the sample S around the sample center X, and a center around the ω axis. And a ω rotation device 8 for rotating the sample S. The sample S is attached to the φ rotating device 6 while being loaded on the sample plate 21. In the case of this embodiment, the arc swing mechanism 7 is mounted on the ω rotating device 8, and the φ rotating device 6 is mounted on the arc swing mechanism 7.
[0028]
As shown in FIG. 4, the sample plate 21 includes a frame member 22 in which a recess 23 is formed, and a single crystal plate 24 provided at the bottom of the recess 23. The frame member 22 is made of, for example, stainless steel, and the single crystal plate 24 is made of, for example, a Si (silicon) single crystal plate. The sample S is loaded into the recess 23 above the single crystal plate 24.
[0029]
The X-ray reading unit T shown in FIG. 3 reflects a support base 11 that supports the photostimulable phosphor 2 in a planar shape, a laser light source 14 that emits laser light, and a laser light emitted from the laser light source 14. A light reflecting member 13a, a scanning optical system 12 that is disposed opposite to the support base 11 and receives light from the light reflecting member 13a, and a laser light detector 16 that receives light from the light reflecting member 13b. Have. The laser light detector 16 includes a photoelectric converter, for example.
[0030]
The scanning optical system 12 is driven by the scanning drive unit 17 to scan the surface of the photostimulable phosphor 2 in two orthogonal directions of XY, that is, in a plane direction. The scanning optical system 17 can be configured using an arbitrary parallel movement mechanism. The laser light detector 16 receives light and outputs a signal corresponding to the light intensity. An X-ray intensity calculation circuit 18 is connected to the output terminal of the laser light detector 16.
[0031]
The arithmetic device 26 has a CPU (Central Processing Unit) 28 and a memory 29. The CPU 28 performs calculations for controlling various devices connected to the bus 27. The memory 29 includes a memory area for storing a program used by the CPU 28, a memory area that functions as a work area for the CPU 28, a temporary file, and the like. Specifically, the memory 29 includes a semiconductor memory, a hard disk, Other various storage media can be used.
[0032]
The X-ray intensity calculation circuit 18 and the scanning drive device 17 are each connected to the CPU 28 through the input / output interface 31. The input / output interface 31 is connected to a CRT or other display 32 for displaying information as an image and a printer 33 for printing information on a printing material such as paper.
[0033]
The operation of the X-ray apparatus comprising the X-ray exposure unit R shown in FIG. 1 and the X-ray reading unit T shown in FIG. 3 will be described below. In the measurement using the X-ray apparatus, first, preliminary measurement is performed on the single crystal plate 24 of the single crystal sample plate 21, and then the main measurement is performed with the sample S loaded on the single crystal sample plate 21, A series of processes is performed in which the final measurement result is obtained by correcting the result of the main measurement with the result of the preliminary measurement. Hereinafter, each process will be described individually.
[0034]
(Preliminary measurement for single crystal sample plate 21)
First, in the X-ray exposure part R of FIG. 1, the cylindrical photostimulable phosphor 2 is installed so that the center axis thereof coincides with the ω axis. Further, a sample plate 21 not loaded with the sample S is attached to a predetermined position of the φ rotation device 6 of the sample support device 1, and the single crystal plate 24, that is, the single crystal sample plate 21 is set to have the same measurement conditions as in the main measurement. Adjust the positional relationship.
[0035]
Specifically, as shown in FIG. 2, the ω rotation device 8 is operated to set the incident angle θ 0 of X-rays with respect to the sample surface of the single crystal sample plate 21 to a predetermined angle, for example, 20 ° to 30 °. Here, the sample surface of the single crystal sample plate 21 is a surface that coincides with the sample surface of the sample S when the sample S is loaded on the single crystal sample plate 21.
[0036]
Next, in FIG. 1, the arc rocking mechanism 7 is operated so that the sample surface of the single crystal sample plate 21 is inclined at an angle θ1 with respect to the central axis of the stimulable phosphor 2 and hence the ω axis, for example, approximately 45 °. Adjust as follows. Although this adjustment is performed manually in this embodiment, it can also be performed automatically by attaching a motor or other drive source to the arc swing mechanism 7.
[0037]
As described above, the sample surface of the single crystal sample plate 21 is inclined at about 45 ° with respect to the photostimulable phosphor 2 when the main measurement is performed on the sample S along the tangential direction from the sample S to the sample surface. This is because both the diffracted X-ray R3 emitted and the diffracted X-ray R4 emitted along the sample vertical direction can be detected by the photostimulable phosphor 2. Therefore, the tangential diffraction X-ray R3 and the vertical diffraction X are obtained even when the tilt angle of the sample surface is deviated from 45 ° due to the long length of the stimulable phosphor 2 in the axial direction (vertical direction in the figure). When both of the lines R4 can be detected by the photostimulable phosphor 2, it is not always necessary to set the angle exactly 45 °.
[0038]
After completion of the above setting, the φ rotating device 6 is operated to rotate the single crystal sample plate 21 and thus the single crystal plate 24 around the φ axis, that is, in-plane rotation, and then radiate from the X-ray focal point F to obtain the monochromator 3. The X-rays that have passed through the collimator 4 are incident on the single crystal plate 24 that rotates in-plane. At this time, if the Bragg diffraction condition is satisfied between the incident X-ray and the crystal lattice plane of the single crystal plate 24, X-ray diffraction occurs in the single crystal plate 24.
[0039]
Since the single crystal plate 24 is formed of a single crystal material, the diffracted X-rays are generated only from a limited portion. Therefore, on the surface of the photostimulable phosphor 2, as shown in FIG. Several diffraction spots are obtained. FIG. 5B shows the relationship between the diffraction points and the diffraction angles. In the figure, {circle over (1)}, {circle around (2)}, {circle around (3)},... Indicate equal diffraction angle lines corresponding to each diffraction point.
[0040]
If the photostimulable phosphor 2 is mounted on the support base 11 of the X-ray reading unit T in FIG. 3 and reading is performed by irradiating laser light while scanning and moving the scanning optical system 12 in the XY plane, The coordinate position of the diffraction point in FIG. 5A, that is, the diffraction X-ray image in the XY plane can be obtained by the calculation of the CPU.
[0041]
The CPU 28 sums, for example, integrates the intensities of the diffracted X-ray images regarding the single crystal plate 24 thus obtained for each equal diffraction angle line, thereby obtaining each diffraction angle (see FIG. 5C). X-ray intensity for every 2θ) can be calculated. In FIG. 5C, {circle over (1)}, {circle around (2)}, {circle around (3)},... Correspond to the equal diffraction angle lines in FIG.
[0042]
In this embodiment, the CPU 28 stores the diffraction X-ray image relating to the single crystal plate 24, that is, the coordinate position of each diffraction point B in the memory 29 (see FIG. 3) as a blank area.
[0043]
(Main measurement for sample S)
Next, as shown in FIG. 4, the sample S is loaded on the single crystal sample plate 21, and the sample plate 21 is attached to a predetermined position of the φ rotation device 6 of FIG. Then, the φ rotation device 6 is operated under the same optical conditions as in the preliminary measurement, and the sample S is emitted from the X-ray focal point F while rotating the sample S around the φ axis, that is, in-plane rotation, and the monochromator 3 and the collimator. The X-rays that have passed through 4 are made incident on the minute portion of the sample S that rotates in-plane. At this time, if the Bragg diffraction condition is satisfied between the incident X-ray and the crystal lattice plane of the sample S, X-ray diffraction occurs in the sample S.
[0044]
Since the X-rays incident on the sample S are limited to a minute part, the number of crystal grains contained in the irradiation field is small. Therefore, the diffracted X-rays generated from these crystal grains travel in a specific diffraction angle direction. Therefore, a zero-dimensional X-ray detector such as SC (scintillation counter) or PSPC (position sensitive proportional counting). In the case of a one-dimensional X-ray detector such as a tube), the X-ray detectors must be scanned, that is, rotated by the χ axis in order to capture the diffracted X-rays. On the other hand, according to the present embodiment, it is possible to perform the same measurement as the conventional rotation about the two axes of the χ axis and the φ axis by simply rotating the sample S without rotating the χ axis.
[0045]
Further, in the conventional method in which the χ axis must be rotated in addition to the φ axis rotation, the spread of the X-ray irradiation field in the sample S is often increased due to the crossing error of these two axes, It was insufficient with respect to irradiating the partial area with high accuracy by X-rays. On the other hand, according to the present embodiment, in which rotation around the χ axis is unnecessary and only one axis rotation around the φ axis is sufficient, it is possible to prevent the X-ray irradiation field from being widened, thereby avoiding a decrease in measurement accuracy. it can.
[0046]
Further, in this embodiment, since one rotational drive system for the sample can be omitted, the structure of the apparatus can be simplified. Furthermore, since a two-dimensional X-ray detector is used, the measurement time can be shortened compared to the case where a zero-dimensional X-ray detector and a one-dimensional X-ray detector are used.
[0047]
When the exposure processing as described above is performed in the X-ray exposure unit R of FIG. 1, the surface of the photostimulable phosphor 2 is exposed by diffracted X-rays from the sample S as shown in FIG. Diffraction points a, b, c,..., F are formed at the positions. Further, the diffraction points shown in FIG. 5A are formed so as to overlap with each other as indicated by “x” corresponding to the diffracted X-rays from the single crystal plate 24 supporting the sample S (see FIG. 4).
[0048]
FIG. 6B shows the relationship between these diffraction points and the equal diffraction angle lines (1), (2), (3),... Shown in FIG. The diffraction points a, b,..., F corresponding to the sample S may be placed on equal diffraction angle lines (1), (2), (3),. .
[0049]
The photostimulable phosphor 2 that has been subjected to the exposure process is subjected to a reading process in the X-ray reading unit T shown in FIG. Then, the CPU 28 in the arithmetic unit 26 individually obtains the XY coordinate position and the X-ray intensity of the diffracted X-ray image formed on the surface of the photostimulable phosphor 2, and further X-rays belonging to the same diffraction angle. The sum of the intensities is obtained by calculation, for example, integration.
[0050]
If the X-ray intensity is integrated with respect to (1), (2), (3),... Or other individual diffraction angles without any correction, FIG. As shown in FIG. 4, when the diffracted X-rays from both the single crystal plate 24 and the sample S have the same diffraction angle, they are added to form a high peak, and the diffraction angle of the diffracted X-ray from the sample S Is different from the diffraction angle of the diffracted X-ray from the single crystal plate 24, a new peak appears at a position different from the equal diffraction angle lines (1), (2), (3),.
[0051]
The X-ray intensity distribution shown in FIG. 6C includes the diffracted X-ray information of the single crystal plate 24, and therefore does not indicate a correct X-ray intensity distribution regarding the sample S. In order to eliminate this inconvenience, the CPU 28 treats the coordinate position set as the blank area B (see FIG. 5) in the previous preliminary measurement as not being included in the above integration calculation, and only the diffracted X-rays from the sample S, etc. Integrate for each diffraction angle line.
[0052]
As a result, the X-ray intensity distribution as shown in FIG. 7, that is, the X-ray intensity distribution corresponding to the overlap distribution curve of FIG. 6C excluding the distribution curve corresponding to the single crystal plate of FIG. Is obtained. The observer can know the crystal structure and the like of the sample S by examining the peak position and peak height in the graph of FIG.
[0053]
As described above, in this embodiment, the diffracted X-rays from the single crystal plate 24 supporting the sample S in FIG. 4 are set as blank regions and excluded from the object of integration calculation. The X-ray intensity distribution can be accurately obtained based only on the diffracted X-rays from the sample S without being affected by the X-rays. Further, there is no decrease in the P / B ratio due to the halo as in the case of using glass as the sample plate.
[0054]
(Other embodiments)
The present invention has been described with reference to the preferred embodiments. However, the present invention is not limited to the embodiments, and various modifications can be made within the scope of the invention described in the claims.
[0055]
For example, in the embodiment of FIG. 1, the measurement is performed in a state where the sample S is inclined by 45 ° with respect to the ω axis, but the sample S can be set at an inclination angle other than 45 °, It is also possible to set the angle to 0, that is, the horizontal state.
[0056]
In the embodiment of FIG. 1, micro X-ray diffraction measurement is performed on the condition that the beam diameter of X-rays irradiated to the sample S is limited to a minute diameter and that the sample S is rotated in-plane around the φ axis. As an example, the present invention is not limited to being applied to such a micro X-ray diffraction measurement, but for any kind of X-ray diffraction measurement in which the sample S needs to be supported by a sample plate. Applicable.
[0057]
Further, the X-ray reading unit T shown in FIG. 3 is merely an example, and various other structures can be adopted as a specific structure.
[0058]
Further, in the embodiment of the single crystal sample plate 21 shown in FIG. 4, the single crystal plate 24 and the frame member 22 are formed separately, but the entire sample plate 21 can be formed only by the single crystal plate 24.
[0059]
Further, the graphs shown in FIGS. 5C, 6C, and 7 are examples for easily showing the diffracted X-ray intensity distribution, and the peak distribution status and the peak height are the types of the sample S. It changes variously according to.
[0060]
Further, in the above embodiment, the preliminary measurement on the single crystal sample plate is performed before the main measurement on the sample is performed. However, if the diffraction angle of the diffraction X-ray on the single crystal sample plate is known in advance, the preliminary measurement is performed. Without performing the measurement, the known diffraction angle information can be input to the arithmetic unit via an input device such as a keyboard, and the input region can be set as a blank region.
[0061]
【The invention's effect】
According to the X-ray apparatus and the X-ray measurement method of the present invention, the sample plate for supporting the sample is formed using a single crystal substance, and therefore, compared to the case where the sample plate is formed using glass. The ground can be reduced and highly accurate measurement can be performed.
[0062]
In addition, since a two-dimensional X-ray detector is used as the X-ray detector, diffraction X-rays can be captured only by rotating the sample in a plane, that is, uniaxially, when the sample is very small. Thus, it is not necessary to rotate the sample in two axes. In a two-axis rotating system, it is difficult to make the intersection of these two axes exactly coincide with one point, so that the area of the X-ray irradiation field on the sample becomes large, and the original measurement purpose of micro-part measurement can be achieved. There is a risk of disappearing. On the other hand, in the present invention, since the rotation system used is only one axis, the X-ray irradiation field on the sample does not widen, and therefore X-rays can be accurately incident only on the minute part to be measured. it can.
[0063]
Furthermore, since the diffracted X-ray generated from the single crystal sample plate is recognized as a blank region and excluded from the calculation, even if X-rays incident on the sample to be measured are incident on the single crystal sample plate, The X-ray diffraction measurement on the sample can be performed very accurately by eliminating the influence of the diffracted X-rays from the plate.
[Brief description of the drawings]
FIG. 1 is a perspective view showing an embodiment of an X-ray exposure unit which is a main part of an X-ray apparatus according to the present invention.
FIG. 2 is a plan view of an X-ray exposure unit in FIG.
FIG. 3 is a perspective view showing an embodiment of an X-ray reading unit which is another main part of the X-ray apparatus according to the present invention.
4 is a side sectional view showing an example of a single crystal sample plate used in the X-ray exposure unit of FIG. 1. FIG.
FIG. 5 is a diagram showing an example of a diffraction X-ray image formed on the surface of a two-dimensional X-ray detector with respect to a single crystal plate, (a) showing only the diffraction X-ray image, and (b) showing the diffraction X-ray image. The relationship between a diffraction X-ray image and an equal diffraction angle line is shown, and (c) shows an X-ray intensity distribution diagram.
FIG. 6 is a diagram showing an example of a diffraction X-ray image formed on the surface of a two-dimensional X-ray detector with respect to both a sample and a single crystal plate supporting the sample, and FIG. (B) shows the relationship between the diffraction X-ray image and the equal diffraction angle line, and (c) shows an X-ray intensity distribution diagram.
7 is a graph showing an example of a diffraction X-ray intensity distribution diagram for only a sample, which is obtained by calculation based on the diffraction X-ray image shown in FIG.
FIG. 8 is a perspective view showing an example of a conventional X-ray apparatus, particularly a conventional micro X-ray diffraction apparatus.
[Explanation of symbols]
1 Sample support device
2 photostimulable phosphor
3 Monochromator
4 Collimator
6 φ rotating device
7 Arc swing mechanism
8 ω rotating device
11 Support stand
12 Scanning optical system
14 Laser light source
16 Laser detector
21 Sample plate
22 Frame member
23 recess
24 Single crystal plate
B Blank area
F X-ray focus
R X-ray exposure unit
S sample
T X-ray reader
X Sample center

Claims (10)

In an X-ray apparatus having an X-ray exposure unit that irradiates a sample with X-rays and detects diffracted X-rays generated from the sample, and an X-ray reading unit that reads diffracted X-rays detected by the X-ray exposure unit,
The X-ray exposure unit is disposed around the sample plate, a single crystal sample plate that is formed of a single crystal material and supports the sample, an X-ray source that emits X-rays toward the sample, and the like. A two-dimensional X-ray detector;
The X-ray reading unit
X-ray reading means for reading the data in the two-dimensional X-ray detector in a plane and outputting it as a signal;
Calculation means for integrating the X-ray intensities belonging to the same diffraction angle based on the output signal of the X-ray reading means to obtain a diffraction X-ray intensity distribution by calculation ;
Storage means for storing a coordinate position at which a diffracted X-ray emitted from the single crystal sample plate is detected by the two-dimensional X-ray detector ;
The X-ray apparatus characterized in that the computing means excludes the coordinate position of diffracted X-rays from the single crystal sample plate stored by the storage means from the integration target . In claim 1,
Φ rotation means for rotating the sample in-plane,
The X-ray exposure unit exposes the two-dimensional X-ray detector with diffracted X-rays emitted from the sample by performing only in-plane rotation of the sample by the φ rotating means. apparatus. 3. The tilt moving means for tilting and moving the sample surface of the sample with respect to the two-dimensional X-ray detector, and rotating the sample to change the X-ray incident angle with respect to the sample. An X-ray apparatus having ω rotating means. In claims 1 one claims 3 Neu Zureka, the two-dimensional X-ray detector is the X-ray apparatus characterized by being formed by a stimulable phosphor. In claims 1 one claim 4 Neu Zureka, the sample surface of the sample, the X-ray apparatus characterized by 45 ° inclined with respect to the central axis of the two-dimensional X-ray detector. The sample is supported by a single crystal sample plate formed of a single crystal material,
Irradiate the sample with X-rays,
Diffracted X-rays generated from the sample are detected by a two-dimensional X-ray detector disposed around the sample;
The coordinates and intensity of the diffracted X-ray detected by the two-dimensional X-ray detector are read by the X-ray reading means, and the X-ray intensities belonging to the same diffraction angle are integrated based on the output signal of the X-ray reading means. An X-ray measurement method for obtaining a diffracted X-ray intensity distribution by calculation by a calculation means,
Storing the coordinate position where the diffracted X-ray emitted from the single crystal sample plate is detected by the two-dimensional X-ray detector in the storage means before the calculation by the calculation means;
The calculation means excludes the coordinate position of the diffracted X-ray from the single crystal sample plate stored by the storage means from the integration target when the calculation is performed by the calculation means. X-ray measurement method. In claim 6,
X-rays are irradiated to a single crystal sample plate in a state where the sample is not supported, and the diffracted X-rays from the single crystal sample plate are detected by the two-dimensional X-ray detector, and the coordinates of the diffracted X-rays obtained at that time are detected. An X-ray measurement method characterized by storing a position in the storage means . 8. The X-ray detector according to claim 6 or 7, wherein the sample is irradiated with X-rays while only rotating the sample in-plane, and the diffracted X-rays generated from the sample are detected by the two-dimensional X-ray detector. X-ray measurement method. In claim 8 Neu Zureka one of claims 6, X-ray measurement method, wherein the two-dimensional X-ray detector is formed by a stimulable phosphor. In the claims 6 to one claim 9 Neu Zureka, the sample surface of the sample, the X-ray measurement method characterized by 45 ° inclined with respect to the central axis of the two-dimensional X-ray detector.

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