JP2008275387A - X-ray single crystal orientation measuring device and measuring method therefor - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an X-ray single crystal orientation measuring device and a measuring method capable of performing highly accurately at high speed, orientation determination of all the three axes for examining the fitting state of a crystal axis with respect to the outer shape of a crystal. <P>SOLUTION: This device has characteristics wherein a diffractometer method utilizing diffraction by a characteristic X-ray is used as a base, and a two-dimensional detector based on CCD operated in a TDI reading-out mode is adopted as an X-ray detector, and orientation determination of all the three axes is performed by capturing at two points, reflection of a specified (aimed) index by the two-dimensional detector. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention relates to an X-ray single crystal orientation measuring apparatus and a measuring method thereof for determining all three-axis orientations for examining how crystal axes are attached to the outer shape of a crystal.

  For all three-axis crystal orientation measurement, a diffractometer method four-axis diffractometer using characteristic X-rays and a Laue method using continuous X-rays have been used.

  An improvement of the diffractometer method using characteristic X-rays is known in JP-A-5-312736 (Patent Document 1). That is, in Patent Document 1, (1) an arbitrary single crystal lattice plane of a single crystal serving as a sample is selected, and a diffraction angle corresponding to the crystal lattice plane is selected with respect to incident X-rays to the sample. And (2) diffracting from the sample by irradiating the sample with incident X-rays and rotating the sample about an axis perpendicular to the incident X-rays. The process of detecting X-rays with the detector and obtaining the rotation angle ω1 of the sample at that time, and (3) detecting the position on the arc-shaped detection surface where the diffracted X-rays hit, Is determined as an angle φ1 from the reference plane including the incident X-ray, and (4) any other crystal lattice plane of the single crystal to be the sample is selected, and the above (1), (2), (3) The process of repeating the process of obtaining the sample rotation angle ω2 and the detection position angle φ2 at that time, 5) ω1, φ1, ω2, X-ray single crystal orientation measuring method and a process of obtaining the orientation of the single crystal sample by calculation using φ2 is been described.

  Japanese Patent Laid-Open No. 58-75051 (Patent Document 2) is known as an improvement of the Laue method using continuous X-rays.

JP-A-5-312736 JP 58-75051 A W.C Hamilton, “International Table for X-ray Crystallography Vol. IV”, Kyonch Press, Birmingham (1974) P274-284

  The above Patent Documents 1 and 2 are applied to turbine blade azimuth measurement. The improvement of the diffractometer method shortens the measurement time to about 1 minute, and the improvement of the Laue method shortens the measurement time to several tens of seconds. Speedup was achieved.

  An object of the present invention is to provide an X-ray single crystal orientation measuring apparatus and measurement capable of determining all three axes of orientation at high speed and with high accuracy to examine how the crystal axes are attached to the outer shape of the crystal. It is to provide a method.

  In order to achieve the above object, the present invention is based on a diffractometer method using diffraction by characteristic X-rays, and based on a CCD operating in a TDI (Time Delay Integration) readout mode as an X-ray detector. X-ray single crystal orientation measuring apparatus and measurement that determine the orientation of all three axes by using the two-dimensional detector and capturing the reflection of a specific (targeted) index at two points by the two-dimensional detector. Is the method.

The present invention also provides an incident X-ray portion that narrows the characteristic X-ray and enters the lattice plane of a single crystal sample at an incident angle ω with respect to the X axis in the XZ axis plane, and the incident angle ω is determined by the diffraction condition. Scanning means for scanning by rotating around the Y axis relatively between the incident X-ray part and the sample so as to change within an appropriate range centering on an incident angle ω ₀ satisfying By scanning at least the incident angle ω incident on the sample from the incident X-ray portion, at least 2 of a specific index emitted along a conical surface having a diffraction angle 2θ obtained from an irradiation point on the lattice plane of the sample An X-ray detector having a two-dimensional detector composed of a CCD operating in a TDI readout mode for capturing a two-dimensional image including images of two diffraction spots, and obtained from the two-dimensional detector of the X-ray detector The two diffraction spots based on the two-dimensional image Incident angle omega _{s 1} each bet has occurred, determine the omega _s 2, the incident angle omega _{s 1} obtained, representing the outer shape of the sample from each of the omega _s 2 (XYZ) of at least 2 in the coordinate system An arithmetic processing unit that calculates normal vectors V1 and V2 of two lattice planes and determines the triaxial crystal orientation of the sample based on the calculated normal vectors V1 and V2 of at least two lattice planes. An X-ray single crystal orientation measuring apparatus characterized by the above.

Further, according to the present invention, in the arithmetic processing unit, each of the incident angles ω _s 1 and ω _s 2 at which each of the two diffraction spots is generated is expressed in the V direction of the two-dimensional image obtained from the two-dimensional detector and It is characterized in that it is obtained by converting to an ω angle based on the pixel address in the W direction.

  According to the present invention, the X-ray detection unit reduces a strip-shaped or bow-shaped fluorescent plate for converting an X-ray image into a visible light image, and a visible light image obtained from the fluorescent plate at least in the V direction. A lens system that forms an image, an image intensifier that multiplies the luminance of a light image formed by the lens system, and a CCD that is coupled to the image intensifier and operates in the TDI readout mode. And an imaging width in the V direction is increased.

  According to the present invention, the X-ray detection unit has a thin band-shaped or bow-shaped fluorescent plate for converting an X-ray image into a visible light image, and forms a visible light image obtained from the fluorescent plate; An image intensifier for multiplying the brightness of the light image formed by the lens system, and a two-dimensional detector composed of a CCD operating in the TDI readout mode coupled with the image intensifier; It is characterized in that at least two channels constituted by are arranged side by side.

  Further, the present invention is characterized in that the shape of the light receiving surface of the two-dimensional detector composed of the CCD operating in the TDI readout mode is formed in a narrow band shape.

The present invention also provides an incident X-ray portion that narrows the characteristic X-ray and enters the lattice plane of a single crystal sample at an incident angle ω with respect to the X axis in the XZ axis plane, and the incident angle ω is determined by the diffraction condition. Scanning means for scanning by rotating around the Y axis relatively between the incident X-ray part and the sample so as to change within an appropriate range centering on an incident angle ω ₀ satisfying By scanning at least the incident angle ω incident on the sample from the incident X-ray part, at least 2 of a specific index emitted along a conical surface having a diffraction angle 2θ obtained from an irradiation point on the lattice plane of the sample Using an X-ray single crystal orientation measuring apparatus including an X-ray detector having a two-dimensional detector configured with a CCD operating in a TDI readout mode, which captures a two-dimensional image including images of two diffraction spots,
Based on the two-dimensional image obtained from the CCD of the X-ray detector, the incident angles ω _s 1 and ω _s 2 generated by the two diffraction spots are obtained, and the obtained incident angles ω _s 1 and ω The normal vectors V1 and V2 of at least two lattice planes in the (XYZ) coordinate system representing the outer shape of the sample are calculated from each of _s2 , and the calculated normal vectors V1 and V1 of the at least two lattice planes are calculated. An X-ray single crystal orientation measuring method characterized in that the triaxial crystal orientation of the sample is determined based on V2.

  Further, the present invention is characterized in that the sample is a grain-oriented silicon steel plate.

  As described above, according to the present invention, for example, a three-axis orientation distribution measurement of a directional silicon steel plate or the like has been speeded up, and a short-time map measurement has become possible.

  Embodiments of an X-ray single crystal orientation measuring apparatus and measuring method according to the present invention will be described with reference to the drawings.

  By the way, single crystals have different mechanical, optical, and electromagnetic properties depending on crystal orientation (there is anisotropy). When actively utilizing such crystal characteristics, it is necessary to examine the crystal orientation. An example of a sample that positively utilizes crystal anisotropy is a grain-oriented silicon steel sheet. Directional silicon steel sheet is a material that is used as an iron core for transformers and the like, and is used for the purpose of significantly reducing iron loss and noise of transformers. In this material, secondary recrystallized grains are formed by rolling and heat treatment. When the individual crystal grains are accumulated in parallel with {110} of the crystal lattice plane and the rolling direction in parallel with the <001> direction, the highest magnetic flux density and low iron loss magnetic characteristics can be obtained. This ideal orientation distribution structure is expressed as {110} <001> and discovered by Goss, so it is called Goss orientation.

  As described above, in the manufacture of grain-oriented silicon steel sheets, since magnetic characteristics and crystal orientation are discussed in association with each other, crystal grain orientation measurement by X-ray is performed in the form of map measurement. And evaluation is added based on the result of orientation measurement, and it is fed back to the setting of rolling conditions and heat treatment conditions.

  In this way, grain oriented silicon steel sheets made with advanced and precise control are said to be “art of iron”. In order to meet the recent strong demands for energy saving and carbon dioxide reduction, research is being continued with the aim of developing products with lower iron loss and higher magnetic flux density. As an evaluation method, orientation measurement by X-rays is performed, but an X-ray single crystal orientation measuring apparatus capable of map measurement at higher speed is demanded.

  An embodiment in which the X-ray single crystal orientation measuring apparatus and measuring method according to the present invention are applied to, for example, a grain-oriented silicon steel sheet as a sample piece (crystal to be measured) 1 will be described. Here, the single crystal sample according to the present invention refers to an aggregate material (substance) whose region is sufficiently composed of a single crystal as compared to X-ray irradiation (about φ1 mm). An example of this sample is a grain-oriented silicon steel plate.

  FIG. 1 shows the orientation relationship of a directional silicon steel sheet with ideal orientation (Goss orientation: {110} <001> structure). The surface normal direction Z-axis is called ND (Normal Direction) and is parallel to the crystal axis [110]. The sample longitudinal direction X-axis is called RD (Rolling Direction) and is parallel to the crystal axis [001]. The transverse Y-axis perpendicular to them is called TD (Transverse Direction) and is parallel to the crystal axis [−110].

  An actual silicon steel sheet is an aggregate of crystal grains of about 5 mm to 30 mm, and there are variations in crystal grain orientation. The amount of variation is about 10 ° around the ideal orientation.

FIG. 1 further shows a specific target by a two-dimensional detector based on a CCD (TDI-CCD) 200 operating in a TDI (Time Delay Integration) readout mode, which is an X-ray detector that is a feature of the present invention. The specific lattice plane normal directions [21-1] and [12-1] that capture the reflection of the index at two points are shown. Diffraction by these reflection surfaces (= lattice surfaces) is called 21-1 reflection and 12-1 reflection. When the characteristic X-rays 13 are incident on the reflecting surface at an incident angle of ω ₀ in the XZ plane, in the case of the ideal orientation, the diffraction conditions are satisfied at the same time on both reflecting surfaces and diffraction lines (diffracted X-rays) are generated simultaneously. In FIG. 1, only the diffraction lines (diffracted X-rays) for 12-1 reflection are shown. When FeKα rays having a wavelength of 1.937 mm are used as characteristic X-rays to be used, the Bragg angle θ of these reflection indices is 55.8 °, and the diffraction angle 2θ is 111.62 °. Further, according to appropriate calculations, the incident angle ω ₀ that satisfies the diffraction conditions is 34.5 °. The direction of the diffraction line (diffracted X-ray) is a direction inclined about 30 ° from the Z-axis, and the angle ε between the X-ray projection line of the diffraction line and the X-axis is 107.3 °. The other diffraction line due to the 21-1 reflection occurs at a mirror symmetry position by the XZ plane. The angle η formed by both diffraction lines is about 57 °.

  Next, a configuration showing an embodiment of an azimuth measuring apparatus using a TDI-CCD will be described with reference to FIG. That is, characteristic X-rays (incident X-rays) 13 generated from a point-shaped X-ray source (not shown) are finely focused by a pinhole collimator 11 having a diameter of about 0.2 to 0.5 mm and irradiated to the sample piece 1. . An Fe target or the like is used as the X-ray source. Although not shown in the figure, a Kβ cut filter is arranged to pseudo-colorize the Kα line. An X-ray detector 20 is arranged in the direction of the diffraction angle (2θ) by a predetermined grating surface, and waits for diffracted X-rays. A two-dimensional detector 200 based on a TDI-CCD is used as the X-ray detector 20. An incident X-ray unit 10 and an X-ray detector 20 including an X-ray source (not shown) and a collimator 11 can rotate together around the Y axis and change the incident angle (ω) of the X-ray. (Ω rotation). The sample piece 1 is placed on an XY stage (not shown), and the position of the X-ray irradiation point can be changed. Of course, instead of rotating the integrated incident X-ray part 10 and X-ray detector 20 around the Y axis, the sample piece 1 may be rotated around the Y axis.

The ω angle is scanned in an appropriate range around ω ₀ . For example, a certain range of about ± 20 ° is scanned. In the configuration of FIG. 2, the TDI readout direction is set in the direction of the equator plane arrow (or vice versa). The equatorial plane is a plane that includes the incident X-ray 13 and is perpendicular to the ω rotation axis (Y axis), and is the XZ axis plane of FIG. When the ω rotation is rotated at a constant speed within a certain range, an instantaneous diffraction line that satisfies the diffraction condition is generated and incident on the TDI-CCD 200. When TDI reading is executed in synchronization with the start and end of ω rotation, two diffraction spots are recorded in the belt-like image 203 as shown in FIG. These two diffraction spots are 21-1 reflection and 12-1 reflection diffraction spots. Specifically, from these positions, as will be described later, all three axial directions ([100], [010] ] (Lattice plane normal vector consisting of [001]).

As shown in FIG. 3, the ω angle is scanned in an appropriate range centering on ω _0, and the longitudinal direction of an image captured by the TDI-CCD 200 has information on the ω angle. it is obvious. Since the number of pixels in the longitudinal direction of the image is related to the scan width of the ω angle, the ω angle per pixel can be obtained. In order to determine the standard of the ω angle, calibration with a standard sample adjusted to the ideal orientation is simple. This is because such a standard sample produces two diffraction spots simultaneously when the ω angle is a predetermined angle. You can also calibrate without using a standard sample. For example, the center of the two-dimensional detector 200 can be mechanically accurately arranged, the 2θ angle can be accurately set, and the number of lines corresponding to the delay from the start of reading to the center of the image can be calibrated in advance. .

  Here, the X-ray diffraction conditions by the sample crystal will be described in more detail with reference to FIG. 4A and 4B are sketches showing the arrangement of the X-ray detection surface 202 and the position of the diffraction spot vector k. The X-ray shows a state where a diffraction spot is captured by the X-ray detection surface 202 arranged in a direction perpendicular to the 2θ direction (U-axis) of the equatorial reflection when the diffraction condition is satisfied by a predetermined grating surface.

  The diffraction line spot vector k always exits along a 2θ cone (conical surface having a diffraction angle 2θ), and generates a diffraction spot on the detection surface 202 of the detector 200. Here, the 2θ cone (conical surface having a diffraction angle 2θ) is a half having an o as a vertex and an x axis (in the opposite direction to the incident X-ray 13) as a rotation axis as shown in FIG. It is a conical surface with an apex angle α. In this case, since the diffraction angle 2θ exceeds 90 °, it is in an inverted umbrella state, so a cone having α as a half apex angle is considered. Here, there is a relationship of α = π−2θ.

  A curved surface obtained by cutting a 2θ cone (conical surface having a diffraction angle 2θ) by the X-ray detection surface 202 is called a conic section or a quadratic curve. A diffraction spot is generated on this curve. This is shown in the TDI-CCD output image 203 shown in FIG. 3 where the diffraction spots are indicated by black circles and the conic curves are indicated by broken lines.

Therefore, an equation of this curve is obtained by the arithmetic processing unit (image processing unit) 30 shown in FIG. As shown in FIGS. 4 and 5, the 2θ cone equation is given by the following equation (1) using the (xyz) coordinates based on the vertex o. However, the x-axis is opposite to the incident X-ray 13. In this way, the (xyz) coordinates with respect to the vertex o are the (XYZ) coordinates set with the rotation axis as the Y axis with respect to the outer shape of the sample piece (crystal) 1, the rotation ω angle around ω ₀ , and It will be set from the relationship. Here, there is a relationship of α = π−2θ.

  As shown in FIGS. 4 and 5, the curve of the cut surface obtained by cutting the 2θ cone at the X-ray detection surface 202 has coordinates (pqr) based on the above equation (1) with o ′ as a reference to the detection surface 202. After conversion, it is obtained by converting to (UVW) coordinates of the detection surface 202 by rotating the coordinates and placing U = 0. The result of the calculation is shown in the following equation (2).

  The shape of the curve calculated using the equation (2) is shown by a solid line 205 in FIG. It is the figure which computed and plotted in the direction of Z direction +/- 100mm when diffraction angle 2theta is 111.62 degrees and camera length L is 100 mm. The diffraction spot always lies on this curve.

Next, a procedure for determining the ω angle at which a diffraction spot caused by 21-1 reflection has occurred will be described with reference to FIG. When the arithmetic processing unit 30 shown in FIG. 2 processes the image 203 recorded in a band shape, the position of the diffraction spot can be known from the address of the pixel. By multiplying this by the effective pixel size, the distance in the V direction and the W direction could be converted. The arithmetic processing unit 30, the distance from ωstart position based on information of omega angle obtained from the control unit 35 for controlling a mechanism for scanning an appropriate range omega corners around the omega ₀ (not shown) W0 I understand. Further, in the arithmetic processing unit 30, Vs is a distance from the equator plane, and Ws is calculated by substituting Vs into the above equation (2). Further, the arithmetic processing unit 30 can convert the W direction into the ω angle based on the ω angle information obtained from the control unit 35. As a result, the arithmetic processing unit 30 converts the distance W0− | Ws | into an angle to obtain Δω. In the arithmetic processing unit 30, the incident angle ω _{s at} which the diffraction spot is generated can be obtained by the following equation (3).

  In FIG. 4, a vector k indicating a diffracted X-ray is expressed by the following equation (4) as a unit vector when expressed in a (U′V′W ′) coordinate system with o as the origin and parallel to (UVW). Can do.

If this is expressed in the (xyz) coordinate system by coordinate transformation and expressed as k _xyz , k _xyz is given by the following equation (5).

On the other hand, k ₀ can be expressed by the following equation (6) with the same (xyz) coordinates.

From k _xyz and k ₀ , the lattice plane normal vector V shown in FIG. 4 can be expressed. Therefore, when the lattice plane normal vector V is handled as a unit vector expressed in (xyz) coordinates and is expressed as V _xyz , the following equation (7) is given.

Next, V _xyz expressed in (xyz) coordinates is converted into V _XYZ expressed in a coordinate system (XYZ) representing the outer shape of the sample (sample piece) 1. V _XYZ expressed in a coordinate system (XYZ) representing the outer shape of the crystal is given by the following equation (8) using ω _s of the above equation (3). In this way, the lattice plane normal vector for 21-1 reflection could be obtained. Since this is the first reflection, V1 is displayed.

  Further, similarly to the image 203 recorded in the band shape, the arithmetic processing unit 30 also appropriately processes the second reflection and the 12-1 reflection to thereby obtain a lattice normal vector for the second reflection. V2 can be obtained.

  In general, the relationship between V and the reflection index of a lattice plane normal vector represented by coordinates (XYZ) representing the outer shape of a sample is handled as follows.

  That is, when (100) is the a axis, [010] is the b axis, and [001] is the c axis (abc) coordinates and the (hkl) lattice plane normal is expressed by the following equation (9): An exponent vector h is introduced.

  As a result, the relationship between V and h can be expressed by the following equation (10).

  U is a matrix of 3 rows and 3 columns, and each element is composed of X, Y, Z axes and direction cosines of a, b, c axes, and represents its own direction. The transformation matrix U of V and h is an orthonormal matrix called an orientation matrix. Once U is determined, the surface normal vector V is determined for all (hkl) by the above equation (10), [100] is the a axis, [010] is the b axis, and [001] is the c axis. The orientation of the sample crystal, which is the exponent vector h representing the (hkl) lattice plane normal in (abc) coordinates, is determined.

  In order to determine U, in principle, three vectors V1, V2, V3 with known non-coplanar (primary independent) indices are required. However, as described in the above-mentioned Patent Document 1 and Non-Patent Document 1, page 280, Section 3.4 Determination of U, the Orientation Matrix, it is possible to process with vectors V1 and V2 whose two indices are known. .

  That is, the method according to the present invention determines all the three-axis directions by obtaining the surface normal vectors V1 and V2 of the two reflections 21-1 and 12-1 included in the TDI-CCD image. is there. In an actual apparatus, as a crystal orientation output, a stereo projection diagram, a pole figure, and Euler angles are displayed on the screen of a display device (not shown) connected to the arithmetic processing unit 30 or the overall control unit (not shown). Can be output.

  Next, TDI reading of the CCD will be described. There is a reading mode called TDI (Time Delay Integration) as a method of reading the CCD. The type of CCD used for the TDI readout is mainly an FFT (Full Frame Transfer) type CCD, and is called an FFT-CCD. In normal FFT readout, first, a subject image is exposed for a certain period of time, and a subject image is accumulated as a charge image in a pixel on the CCD. Next, the exposure is interrupted, and readout is performed during that time. Reading is a method of reading all pixels at once for one screen. The size of the obtained image is also the pixel size. For example, 512 × 512 pixels. In normal FFT readout, if the exposure time is longer than the moving speed of the subject, the subject image is dispersed in a plurality of pixels in the moving direction, resulting in image blurring. In contrast, TDI reading does not have this inconvenience.

  Also, TDI readout is a method in which image accumulation (exposure = charge accumulation) on the CCD and pixel reading for the bottom row are continuously performed. Each row of read data is stored in the memory, and all the remaining signals in the CCD pixels are shifted down by one row. If this operation is repeated continuously, the stored image (charge) repeats movement (charge transfer) every time it is read out. If the charge transfer rate is synchronized with the scan speed of the above-mentioned ω angle, the image is not blurred and the same image is added, so that the signal intensity is enhanced. The obtained image exceeds the pixel size and has a certain width, for example, a 512 pixels width, and can be taken long in a band shape for the duration of the TDI operation. In other words, you can do “panning”. That is, the TDI readout CCD according to the present invention performs a TDI readout operation in synchronization with the ω scan. Then, as shown in FIG. 3, the feature is that angle information (ω angle) is provided in the longitudinal direction of the image extending in a strip shape.

  Next, an example of a specific structure of the above-described X-ray detector 20 will be described with reference to FIGS. The X-ray detector 20 according to the present invention is highly sensitive and needs to capture reflections (diffraction spots) of a specific target index by one ω scan at two points. In the first embodiment shown in FIG. 7, the X-ray detector 20a includes a fluorescent screen 21 that converts an X-ray image into a visible light image, and an image intensifier (II) that converts the visible light image converted by the fluorescent screen 21. A lens system 22 for forming an image on the face plate 23; An image intensifier (II) 23 that multiplies the brightness of the formed visible light image by several tens of thousands by connecting an I power source 24, and the image intensifier (II) 23 increases the luminance. A TDI-CCD 200 that captures a doubled optical image by coupling with a fiber, a lens, or the like is provided in a dark box 25 that is tapered. Connection with the CPU (arithmetic processing unit) 30 is made via the image capturing board 27.

  In particular, in order to capture reflection (diffraction spot) of a specific target index by one ω scan at two points, the dimensions of the fluorescent screen 21 are about 200 mm in length (L) and about 20 mm in width (S). It is formed in a band shape, and is configured such that an image is reduced in the V direction by a lens system 22 provided between the fluorescent plate 21 and the image intensifier (II) 23. More preferably, the fluorescent plate 21 should have a bow shape along the conic curve 205. In this case, S can be about 5 mm.

  The TDI-CCD 200 is preferably a strip-shaped element having a vertical / horizontal pixel ratio of about 10: 1 in accordance with the shape of the fluorescent screen 21. Specifically, a pixel having 1024 × 128 pixels and a pixel size of about 15 μm is used.

  As described above, by configuring the X-ray detector 20a, the imaging width in the V direction can be widened, and two diffraction spots can be reliably placed in the imaging field.

  The entire X-ray detector 20a is arranged in a dark box 25 that is shielded from light. However, as shown in FIG. 7A, the tip is slim (tapered) and the sample 1 is scanned with the sample 1 by ω scanning. There is also a need to avoid interference.

  In the second embodiment shown in FIG. 8, the fluorescent plate 21 constituting the X-ray detector 20b is formed in a band shape or a bow shape, and the lens 22, I.V. I23 and TDI-CCD 200 were configured with at least two channels in the V direction. As a result, for each channel, it is possible to capture and capture the reflection (each diffraction spot) of each specific target index. According to the second embodiment, the reduction ratio of the lens 22 can be reduced by using two channels.

It is a figure which shows the generation | occurrence | production condition of the diffraction X-ray when the ideal azimuth | direction of the grain-oriented silicon steel plate which concerns on this invention, and characteristic X-rays are made to inject into (omega) ₀ . 1 is a schematic configuration perspective view showing an embodiment of an X-ray single crystal orientation measuring apparatus according to the present invention. It is a figure which shows the image which picked up the two diffraction spots which generate | occur | produce when the incident characteristic X-ray based on this invention (omega | ohm) scan was carried out with respect to the sample with the two-dimensional detector based on TDI-CCD. . It is a figure which shows the positional relationship of the 2theta cone which concerns on this invention, and the diffraction spot caught with a two-dimensional detector. It is a figure which shows the definition of the coordinate in the detection surface with respect to the sample surface which concerns on this invention. It is a figure which shows the relationship between the cone curve and the position of the diffraction spot of 21-1 reflection in the image captured (imaged) with the two-dimensional detector based on TDI-CCD which concerns on this invention. It is a figure which shows the specific 1st Example of the X-ray detector which concerns on this invention. It is a figure which shows the specific 2nd Example of the X-ray detector which concerns on this invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 ... Sample piece (crystal to be measured), 10 ... Incident X-ray part, 11 ... Collimator, 13 ... Incident X-ray (incident characteristic X-ray), 20, 20a, 20b ... X-ray detector, 21 ... Fluorescent plate, 22 ... Lens system, 23... Image intensifier (II), 24. I power source, 25 ... dark box, 30 ... CPU (arithmetic processing unit), 35 ... control unit, 200 ... TDI-CCD (two-dimensional detector), 202 ... X-ray detection surface, 203 ... image, 205 ... conical curve.

Claims (7)

An incident X-ray portion that narrows the characteristic X-ray and enters the lattice plane of the single crystal sample at an incident angle ω with respect to the X axis in the XZ axis plane;
Scanning is performed by relatively rotating around the Y axis between the incident X-ray part and the sample so that the incident angle ω changes within an appropriate range around the incident angle ω ₀ satisfying the diffraction condition. Scanning means;
A specific index emitted along a conical surface having a diffraction angle 2θ obtained from an irradiation point on the lattice plane of the sample while scanning the incident angle ω incident on the sample from the incident X-ray portion by the scanning means. An X-ray detector having a two-dimensional detector composed of a CCD operating in a TDI readout mode for capturing a two-dimensional image including images of at least two diffraction spots;
Based on the two-dimensional image obtained from the two-dimensional detector of the X-ray detector, the incident angles ω _s 1 and ω _s 2 generated by the two diffraction spots are obtained, and the obtained incident angle ω _{s is obtained.} 1, normal vectors V1 and V2 of at least two lattice planes in the (XYZ) coordinate system representing the outer shape of the sample are calculated from each of ω _s 2, and the calculated normal lines of the at least two lattice planes An X-ray single crystal orientation measuring apparatus comprising: an arithmetic processing unit that determines a triaxial crystal orientation of the sample based on vectors V1 and V2. In the arithmetic processing unit, each of the incident angles ω _s 1 and ω _s 2 generated by the two diffraction spots is used as a pixel address in the V direction and W direction of the two-dimensional image obtained from the two-dimensional detector. 2. The X-ray single crystal orientation measuring apparatus according to claim 1, wherein the X-ray single crystal orientation measuring apparatus is configured to convert the angle into a ω angle based on the obtained angle.   The X-ray detection unit includes a strip-shaped or bow-shaped fluorescent plate that converts an X-ray image into a visible light image, and a lens system that forms a visible light image obtained from the fluorescent plate by reducing the image in at least the V direction. An image intensifier for multiplying the brightness of the light image formed by the lens system, and a two-dimensional detector composed of a CCD operating in the TDI readout mode coupled with the image intensifier; The X-ray single crystal orientation measuring apparatus according to claim 1, wherein:   The X-ray detection unit includes a thin band-shaped or bow-shaped fluorescent plate that converts an X-ray image into a visible light image, and forms a visible light image obtained from the fluorescent plate with a lens system. A channel composed of an image intensifier for multiplying the brightness of the imaged light image and a two-dimensional detector composed of a CCD operating in the TDI readout mode coupled with the image intensifier. The X-ray single crystal orientation measuring apparatus according to claim 1, wherein at least two are arranged side by side.   5. The X-ray single crystal orientation measuring apparatus according to claim 3, wherein a light receiving surface of a two-dimensional detector composed of a CCD operating in the TDI readout mode is formed in a narrow band shape. An incident X-ray portion that narrows the characteristic X-ray and enters the lattice plane of the single crystal sample at an incident angle ω with respect to the X axis in the XZ axis plane, and an incident angle ω that satisfies the diffraction condition. Scanning means for scanning by rotating around the Y axis relatively between the incident X-ray part and the sample so as to change within an appropriate range centering on ₀ , and the incident X-ray part by the scanning means The images of at least two diffraction spots having specific indices emitted from the irradiation point on the lattice plane of the sample along the conical surface of the diffraction angle 2θ while scanning the incident angle ω incident on the sample from Using an X-ray single crystal orientation measuring device including an X-ray detector having a two-dimensional detector configured with a CCD operating in a TDI readout mode for capturing a two-dimensional image including
Based on the two-dimensional image obtained from the two-dimensional detector of the X-ray detector, the incident angles ω _s 1 and ω _s 2 generated by the two diffraction spots are obtained, and the obtained incident angle ω _{s is obtained.} 1, normal vectors V1 and V2 of at least two lattice planes in the (XYZ) coordinate system representing the outer shape of the sample are calculated from each of ω _s 2, and the calculated normal lines of the at least two lattice planes A method for measuring an X-ray single crystal orientation, wherein a triaxial crystal orientation of the sample is determined based on vectors V1 and V2.   The X-ray single crystal orientation measuring method according to claim 6, wherein the sample is a grain-oriented silicon steel plate.

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