JPH06265489A - X-ray diffractometer - Google Patents

Abstract

PURPOSE:To provide an X-ray diffractometer that is able to analyze an orientation property of crystal grains speedily by way of performing the measurement and analysis of an X-ray diffraction pattern. CONSTITUTION:This X-ray diffractometer is made up of installing a sample stage 9 provided with a sample rotary mechanism 8 holding a measured sample 4 and rotating this sample around at least an incident X-ray, an X-ray source 1 applying a white X-ray to the sample 4 at a specified incident angle, an X-ray detector 6 measuring a diffractive X-ray 5 to be diffracted out of the sample 4 and outputting it, and a computer 12 controlling each part, and operating a diffracting angle 2theta from the measured value out of the X-ray detector 6, compounding a turning angle phi of the sample 4 and this diffracting angle 2theta of the diffractive X-ray 5, and making an X-ray diffraction diagram respectively.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an X-ray diffractometer for evaluating materials using X-rays as a probe, and in particular, to rapidly analyze the orientation of crystal grains in various industrial materials and electronic materials. An X-ray diffractometer suitable for

[0002]

2. Description of the Related Art In the prior art, for example, B.I. D. "The X-ray Diffraction Principles" by BD Cullity ("
ELEMENTS OF X-RAY DIFFRAC
Tion ", translated by Gentaro Matsumura, Agne Co., 1972, p. 219, white X-rays are incident on the sample, and the back reflection emitted from the sample is detected by an X-ray film. After developing, the position of the spots of Laue recorded on the film was adjusted to
It was read using a ruler for coordinate axis conversion such as a ger chart and plotted on a stereo projection diagram using a Wulff net or the like to analyze the crystal grain orientation.

Also, for example, Photon Factory Activity Report # 9 ("PHOTON FAC
TORY ACTIVITY REPORT # 9 ",
KEK Progress Report 91-2
A / M, Institute of High Energy Physics, Ministry of Education, 1992
Pp. 137), a monochromatic X-ray is made incident on the sample, the diffracted X-ray pattern from the sample is accumulated on the two-dimensional X-ray detection element, and the two-dimensional image is read by a reading device using a He-Ne laser. Techniques for automatically reading data and obtaining X-ray diffraction patterns have been shown.

[0004]

However, in the technique described in the document "X-ray Diffraction Principles" among the above-mentioned conventional techniques, since a film is used as the X-ray detection element, the development,
A process such as fixing is required, and data processing such as position reading of Laue spots and stereo projection needs to be performed manually using a ruler or the like, which is a problem in terms of speeding up and automation.

Another document, "PHOTOFACT"
In the conventional technique described in "ORY ACTIVITY REPORT # 9", two-dimensional diffraction intensity information can be accumulated and automatically converted into numerical data by using a reading device incorporated in the diffracting device. However, since monochromatic X-rays are used, there is a problem that an optical element such as a monochromator is required and that the light amount of X-rays decreases in the process of monochromaticization. Further, there are problems that the structure of the reading device is complicated and expensive, and that reading takes time. Moreover, the results obtained were essentially the same as when using the film, and the orientation analysis was performed manually.

An object of the present invention is to solve the above-mentioned problems of the prior art. X-ray diffraction which can automatically measure and analyze the X-ray diffraction pattern and rapidly analyze the orientation of crystal grains. To provide a device.

[0007]

The object is to irradiate the sample with a white X-ray at a predetermined incident angle, and a sample stage equipped with a mechanism for holding the sample to be measured and rotating at least around the incident X-ray. An X-ray source, an X-ray detector that measures and outputs diffracted X-rays diffracted from the sample, controls each of the above parts, and calculates a diffraction angle from the measured value from the X-ray detector, And a computer that creates an X-ray diffraction pattern by synthesizing the rotation angle and the diffraction angle of the diffracted X-ray.

Further, the object is to mount a mechanism for rotating around the incident X-rays and a mechanism for moving the sample X-rays in three dimensions with respect to the incident X-rays. As a result, a position sensitive detector capable of simultaneously measuring a plurality of diffracted X-rays from the sample is provided.

Further, the above object is an X-ray detector having an X-ray condensing element for condensing an incident X-ray beam.
Achieved by deploying a line detector.

Still further, the above-mentioned object is to provide a sample stage, an X-ray source, an X-ray detector, a mechanism for rotating the sample stage around an incident X-ray, and a mechanism for moving the sample X-ray in a three-dimensional direction. And a mechanism for rotating the sample stage around the incident X-rays and a mechanism for moving the sample stage in a three-dimensional direction with respect to the incident X-rays.
This is achieved by being configured to be operable from outside the vacuum measuring container.

The above-mentioned object is to have a computer store a function of storing X-ray diffraction information of a known substance, an X-ray diffraction pattern calculation function of calculating an X-ray diffraction pattern from the stored X-ray diffraction information, and measurement. By comparing the X-ray diffraction pattern obtained with the X-ray diffraction pattern obtained by the above calculation with a substance determination function for determining the substance identification of the sample to be measured, the computer can be further preliminarily stored in advance. Input measured sample X
The X-ray diffraction pattern calculation function for calculating the X-ray diffraction pattern from the line diffraction information, and the measured X-ray diffraction pattern and the X-ray diffraction pattern obtained by the calculation are compared to obtain the crystal grain orientation of the sample to be measured. It is achieved by having a crystal grain orientation analysis function for analyzing.

[0012]

The present invention comprises a sample stage, a mechanism for rotating the sample stage around incident X-rays, an X-ray source, an X-ray detector, and a computer. Then, the sample to be measured is held on the sample table, and the surface of the sample is irradiated with white X-rays from the X-ray source at a predetermined angle. White X illuminated on the surface of the sample
The rays diffract to the x-ray detector. When the diffracted X-ray is incident from the sample, the X-ray detector measures the diffracted X-ray and outputs it to the computer. On the other hand, the sample stage is rotated through a mechanism that rotates the sample stage around the incident X-ray, and the sample is rotated with the incident X-ray as a rotation axis. The computer controls the rotation angle φ of the sample in increments of 0.1 °, for example, and at the same time reads the rotation angle φ and inputs the measured value of the diffracted X-rays output from the X-ray detector at this time to perform diffraction. The diffraction angle 2θ of the X-ray is calculated. Then, the computer synthesizes the rotation angle φ of the sample with the incident X-ray as the rotation axis and the rotation angle 2θ of the diffracted X-ray to obtain the Laue spot positions x and y, and X
Create a Laue pattern as a line diffraction pattern.

As a result, according to the present invention, it is possible to automatically measure and analyze the X-ray diffraction pattern and quickly analyze the orientation of the crystal grains of the sample to be measured.

Further, in the present invention, in addition to a mechanism for rotating the sample stage around the incident X-ray, a mechanism for moving the sample stage in a three-dimensional direction with respect to the incident X-ray is attached. As a result, the sample to be measured held on the sample table can be rotated about the incident X-ray as a rotation axis, and the incident position of the incident X-ray on the surface of the sample can be moved and adjusted, so that accurate measurement can be performed. It becomes possible to obtain data.

Furthermore, in the present invention, a position sensitive detector is provided as the X-ray detector, and a plurality of diffracted X-rays from the sample are simultaneously measured by utilizing the characteristics of this position sensitive detector. It becomes possible.

Furthermore, in the present invention, an X-ray detector having an X-ray condensing element is provided as the X-ray detector, and the X-ray condensing element condenses the incident X-ray beam from the sample. I am trying to do it. Therefore, according to the present invention, highly accurate measurement data regarding X-ray detection can be obtained.

Further, in the present invention, the sample stage, a mechanism for rotating the sample stage and a mechanism for moving the sample stage in a three-dimensional direction,
The X-ray source and the X-ray detector are housed in a vacuum measuring container provided with a vacuum exhaust means. A mechanism for rotating the sample table and a mechanism for moving the sample table in three dimensions can be operated from outside the vacuum measurement container. As a result, in the present invention, since X-ray detection can be performed in a vacuum atmosphere, more accurate measurement data can be obtained.

Further, in the present invention, the computer is
A function of storing X-ray diffraction information of a known substance, an X-ray diffraction pattern calculation function of calculating an X-ray diffraction pattern from the stored X-ray diffraction information, and a calculation of the measured X-ray diffraction pattern. It has a substance judging function for judging the substance identification of the sample to be measured by comparing it with the obtained X-ray diffraction pattern. As a result, the orientation of the crystal grains of the sample to be measured can be analyzed more rapidly.

In the present invention, the computer is
An X-ray diffraction pattern calculation function for calculating an X-ray diffraction pattern from the X-ray diffraction information of the sample to be measured, which has been input in advance, and the measured X-ray diffraction pattern and the X-ray diffraction pattern obtained by the calculation are compared. , And a crystal orientation analysis function for analyzing the crystal orientation of the sample to be measured. As a result, also in the present invention, the orientation of the crystal grains of the sample to be measured can be analyzed more quickly.

[0020]

Embodiments of the present invention will be specifically described below with reference to the drawings.

(1) Structure of the X-ray Diffraction Apparatus of the Present Invention FIG. 1 is a side view showing the outline of one embodiment of the present invention.

In the embodiment shown in FIG. 1, an X-ray source 1 and
Collimator 2, sample stage 9 holding sample 4, X, Y stage 7 of sample stage 9, Z stage (not shown) of sample stage 9, rotation mechanism 8 of sample stage 9, X-ray detection Vessel 6,
And a counting system including a computer (see reference numeral 12 in FIG. 2). With the X, Y stage 7 and the Z stage,
A mechanism for moving the sample table 9 in the three-dimensional direction with respect to the incident X-ray 3 is configured.

In this embodiment, the white X-rays generated by the X-ray source 1 are shaped by the collimator 2 and made incident on the sample 4. As the X-ray source 1, a sealed X-ray tube is used in this embodiment, but a rotating anticathode type, a synchrotron radiation type or the like may be used. The sample 4 is mounted on the surface of the sample table 9 placed perpendicularly to the incident X-ray 3 by using a fixing wax or a vacuum chuck. On the sample table 9,
A Z stage is incorporated so that regardless of the shape and thickness of the sample 4, the sample surface can be adjusted so as to be placed at a predetermined position. The sample table 9 is attached to the X, Y stage 7, and the X, Y stage 7 is attached to the sample rotating mechanism 8. With the X and Y stage 7,
The incident position of the incident X-ray 3 on the surface of the sample 4 can be moved, and the incident X-ray 3 can be moved by the sample rotating mechanism 8.
The sample 4 can be rotated around the rotation axis.

Although not shown in the drawing, the rotation mechanism 8, the X, Y stage 7 and the Z stage of the sample table 9 are driven by a motor control circuit and further controlled by a computer 12.

The diffracted X-rays 5 diffracted by the sample 4 are X-rays.
It is measured by the line detector 6. In the case of this embodiment, the curved position-sensitive X-ray detector is used, but a linear detector may be used. In this embodiment, the back reflection Laue spots are arranged to be measured, and the measurable diffraction angle 2θ is 100.
It is from 0 ° to 170 °.

By using a position sensitive detector as the X-ray detector 6, a plurality of diffracted X-rays 5 from the sample 4 can be simultaneously measured.

FIG. 2 is a block diagram of the X-ray detector and counting system in one embodiment of the present invention.

In the embodiment shown in FIG. 2, the X-ray detector 6
An ordinary position-sensitive proportional counter is used as. This position-sensitive proportional counter has a detector container 30 having an X-ray entrance window 31, a working gas enclosed in the detector container 30, an anode line 32 and a delay line 33 stretched in the detector container 30,
It is composed of a high voltage power supply 20 for the anode wire.

Therefore, a positive high voltage is applied to the anode wire 32 stretched in the detector container 30 filled with the working gas when the detector container 30 is set to the ground potential. When the diffracted X-rays 5 enter through the X-ray entrance window 31, the working gas is ionized, and the electrons move toward the anode line 32 and the ions move toward the detector container 30 while amplifying the gas. At the same time, a signal pulse is excited on the delay line 33 and propagates in both directions of the delay line 33. The output of the signal pulse at both ends of the delay line 33 is amplified by the amplifier 22, noise is removed by the wave height analyzer 23, and then input to the time / wave height converter 25. However, the output on one side is input to the time / peak converter 25 after passing through the delay circuit 24. By the above-described signal processing, the incident position of the diffracted X-ray 5 on the X-ray detector 6 is converted into the pulse height of the pulse, which becomes the output of the time / wave height converter 25. The peak value is digitized by the A / D converter 26 and then processed by the multi-channel analyzer 29. Now, the value to be obtained is the X-ray incident position, but directly the output of the multi-channel analyzer 29 is the intensity I (n) of the diffracted X-ray 5 as a function of the channel n. The intensity I (n) of the diffracted X-ray 5 is calculated by the computer 12
Entered in.

The output of the anode line 32 is amplified by the amplifier 22, and the rate meter 28 and the A / D converter 27 are used.
Entered in. Unlike the output of the delay line 33, the output of the A / D converter 27 has no position resolution, but shows the integrated value of the incident intensity of the diffracted X-rays 5 in the entire angular range of the X-ray detector 6. . By looking at the meter of the rate meter 28, the intensity of the diffracted X-ray 5 over the entire angular range can be monitored in real time. At the same time, A
The digitized value input to the / D converter 27 is input to the computer 12. As a result, control can be performed in synchronization with the rotation angle of the sample 4.

(2) Method of measuring diffracted X-rays by the X-ray diffractometer of this embodiment FIG. 3 shows the principle of measuring back reflection Laue spots using this embodiment.

The measurement procedures (a) to (d) shown below are
It is automatically executed and measured by using the computer 12.

(A) The sample 4 is rotated about the incident X-ray 3 as a rotation axis, the rotation angle at that time is φ, and the rotation angle φ is rotated at regular intervals, for example, in 0.1 ° increments, while the anode wire is rotated. Monitor the output of 32. That is, the A / D converter 27
Read the output of.

(B) When this count value exceeds a preset threshold value, the rotation of the sample 4 is stopped and the output of the A / D converter 26 is accumulated in the multi-channel analyzer 29 for a fixed time, for example, 2 seconds. After that, it is transferred to the computer 12.

(C) The computer 12 records the rotation angle φ and the output data of the multi-channel analyzer 29, that is, I (φ, n) in a storage medium such as a magnetic disk.

(D) (a) to (c): 0 ° <φ <360
Do in the range of °.

(3) Method for synthesizing Laue photograph FIG. 4 is a principle diagram for explaining a virtual film and Laue spots incident on its surface.

A Laue photograph can be obtained by performing the following calculations (e) to (g) at the same time as the measurement is performed by the procedure described in (2) above.

(E) The diffraction angle 2θ can be obtained from the number of channels n by the following equation 1.

[0040]

[Equation 1]

However, k and Δn are constants determined by the gain of the amplifier 22 and the arrangement of the X-ray detector 6, and can be obtained in advance using a standard sample or the like.

As a result, I obtained in (c) above
(Φ, n) is converted to I (φ, θ).

(F) The position (x, y) of the Laue spot 11 on the surface of the virtual film 10 is expressed by the following equations 2 and 3.

[0044]

[Equation 2]

[0045]

[Equation 3]

Here, D is the distance (mm) between the sample 4 and the film 10, and x and y are the coordinates (mm) of the Laue spot 11 on the film 10.

(G) From the above, I (φ, θ) is changed to I (x,
y). The combined back reflection Laue photograph can then be output to an output device of the computer 12, such as a CRT or printer.

(4) Stereo Projection As described above, the position of the Laue spot 11 has a diffraction angle of 2
It is represented by θ and the rotation angle φ of the sample 4, but since the white X-rays are used as the incident X-rays 3, the wavelength of the X-rays that contributed to the diffraction is undetermined, and it is not possible to obtain the spacing between the reflecting surfaces. Can not. However, the direction of the normal line of the reflecting surface that forms the Laue spot 11 can be obtained from the position of the Laue spot 11 regardless of the wavelength by (h) described below.

(H) In order to easily know the angular relationship between the reflecting surfaces, it is convenient to use the conformal stereo projection which holds the angular relationship. Generally, if a Wulff net, which is a kind of conformal stereo projection, is used, the angular coordinates of the reflecting surface can be easily plotted.

FIG. 5 is a principle diagram for explaining the relationship between Laue spots and angular coordinates.

Angular coordinates δ and γ on the Wulff net
Is calculated by the following equations 4 and 5.

[0052]

[Equation 4]

[0053]

[Equation 5]

As a result, I (φ, θ) is changed to I (δ, γ)
Convert to.

As described above, the back reflection Laue photograph and the conformal stereo projection can be easily combined from the intensity data of the diffracted X-rays measured by the X-ray diffractometer of this embodiment. This makes it possible to quickly analyze the crystal grain orientation.

(5) Other Embodiments of the Present Invention In the present invention, as the X-ray detector 6, an X-ray focusing element for focusing the incident X-ray beam may be used.

Further, according to the present invention, the sample stage, a mechanism for rotating the sample stage and a mechanism for moving the sample stage in a three-dimensional direction,
An X-ray source and an X-ray detector are housed in a vacuum measurement container provided with a vacuum exhaust means, and a mechanism for rotating the sample table and a mechanism for moving the sample table in a three-dimensional direction are provided from the outside of the vacuum measurement container. It may be operable. By doing so, since X-ray detection can be performed in a vacuum atmosphere, more accurate measurement data can be obtained.

Further, in the present invention, the computer is
A function of storing X-ray diffraction information of a known substance, an X-ray diffraction pattern calculation function of calculating an X-ray diffraction pattern from the stored X-ray diffraction information, and a calculation of the measured X-ray diffraction pattern. The obtained X-ray diffraction pattern may be compared with a substance determination function for determining the substance identification of the sample to be measured. By doing so, the orientation of the crystal grains of the sample to be measured can be analyzed more rapidly.

Furthermore, according to the present invention, an X-ray diffraction pattern calculation function for calculating an X-ray diffraction pattern from the X-ray diffraction information of the sample to be measured, which has been input in advance to the computer, the measured X-ray diffraction pattern and the calculation. A crystal orientation analysis function of analyzing the crystal orientation of the sample to be measured by comparing it with the X-ray diffraction pattern obtained in this manner may be provided. By doing so, the orientation of the crystal grains of the sample to be measured can be analyzed more rapidly.

[0060]

Advantageous Effects of Invention (Claim 1) A sample to be measured is held and at least incident X
A sample stage having a mechanism for rotating around a line, an X-ray source for irradiating the sample with white X-rays at a predetermined incident angle, and an X-ray detection for measuring and outputting diffracted X-rays diffracted from the sample And a computer for controlling the above-mentioned respective parts, calculating a diffraction angle from the measured value from the X-ray detector, synthesizing the rotation angle of the sample and the diffraction angle of the diffracted X-ray, and creating an X-ray diffraction pattern. Since it is configured to include and, the X-ray diffraction pattern is automatically measured and analyzed, and the orientation of the crystal grains of the sample to be measured can be quickly analyzed.

(Claim 2) Since a mechanism for rotating around the incident X-rays and a mechanism for moving the incident X-rays in a three-dimensional direction are attached to the sample table, the sample table is held. Since the sample to be measured can be rotated about the incident X-ray as a rotation axis and the incident position of the incident X-ray on the surface of the sample can be moved and adjusted, accurate measurement data can be obtained.

(Claim 3) As the X-ray detector, a position-sensitive detector capable of simultaneously measuring a plurality of diffracted X-rays from a sample is provided, and the characteristics of this position-sensitive detector are utilized. , There is an effect that a plurality of diffracted X-rays from the sample can be simultaneously measured.

(Claim 4) An X-ray detector having an X-ray condensing element is provided as the X-ray detector, and the X-ray condensing element condenses the incident X-ray beam from the sample. Therefore, there is an effect that highly accurate measurement data regarding X-ray detection can be obtained.

(Claim 5) A vacuum provided with a vacuum exhaust means for the sample stage, a mechanism for rotating the sample stage and a mechanism for moving the sample stage in three dimensions, an X-ray source and an X-ray detector. A mechanism for rotating the sample table and a mechanism for moving the sample table in a three-dimensional direction while being housed in the measurement container are configured to be operable from outside the vacuum measurement container, and X-ray detection can be performed in a vacuum atmosphere. There is an effect that more accurate measurement data can be obtained.

(Claim 6) A function of storing X-ray diffraction information of a known substance in the computer and the stored X
The X-ray diffraction pattern calculation function for calculating the X-ray diffraction pattern from the line diffraction information and the measured X-ray diffraction pattern and the X-ray diffraction pattern obtained by the calculation are compared to identify the substance of the sample to be measured. Since it has the function of judging the substance to be judged, there is an effect that the orientation of the crystal grains of the sample to be measured can be analyzed more rapidly.

(Claim 7) An X-ray diffraction pattern calculation function for calculating an X-ray diffraction pattern from the X-ray diffraction information of the sample to be measured, which has been input in advance to the computer, and the calculated X-ray diffraction pattern. Since it has a crystal orientation analysis function for analyzing the crystal orientation of the sample to be measured by comparing it with the X-ray diffraction pattern obtained as described above, in the present invention as well, the crystal grain of the sample to be measured can be more rapidly measured. The orientation can be analyzed.

[Brief description of drawings]

FIG. 1 is a side view showing an outline of an embodiment of the present invention.

FIG. 2 is a block diagram showing an X-ray detector and a counting system according to an embodiment of the present invention.

FIG. 3 is a principle diagram of measurement of back reflection Laue spots using an embodiment of the present invention.

FIG. 4 is a principle diagram illustrating a method for synthesizing Laue photographs.

FIG. 5 is a principle diagram illustrating a relationship between Laue spots and angular coordinates.

[Explanation of symbols]

1 ... X-ray source, 2 ... Collimator, 3 ... Incident X-ray, 4 ... Sample, 5 ... Diffraction X-ray, 6 ... X-ray detector, 7 ... X, Y stage, 8 ... Sample rotation mechanism, 9 ... Sample stand 10 ... film,
11 ... Laue spots, 12 ... Computer, 20 ... High-voltage power supply, 30 ... Detector container, 31 ... X-ray entrance window, 32 ... Anode line, 33 ... Delay line.

─────────────────────────────────────────────────── ───

[Procedure amendment]

[Submission date] April 9, 1993

[Procedure Amendment 1]

[Document name to be amended] Statement

[Name of item to be corrected] Claim 4

[Correction method] Change

[Correction content]

[Procedure Amendment 2]

[Document name to be amended] Statement

[Correction target item name] 0009

[Correction method] Change

[Correction content]

Furthermore, the object is by the deployment of the X-ray focusing device for focusing the incoming morphism X-ray beam is achieved.

[Procedure 3]

[Document name to be amended] Statement

[Correction target item name] 0016

[Correction method] Change

[Correction content]

Furthermore, in the present invention, the incident X-rays are collected.
The X-ray focusing device for light has deployment, incident on the sample
The X-ray beam is focused. Therefore, according to the present invention , highly accurate measurement data can be obtained in a minute area on the sample surface .

[Procedure amendment 4]

[Document name to be amended] Statement

[Name of item to be corrected] 0023

[Correction method] Change

[Correction content]

In this embodiment, the white X-rays generated by the X-ray source 1 are shaped by the collimator 2 and made incident on the sample 4. As X-ray source 1, in this embodiment uses a sealed X-ray tube, it may be used rotating anode type X-ray tube or synchrotron radiation light and the like. Sample 4 is incident X-ray 3
It is mounted on the surface of the sample table 9 placed vertically with respect to the surface using a fixing wax or a vacuum chuck. A Z stage is incorporated in the sample stage 9 and can be adjusted so that the sample surface is placed at a predetermined position regardless of the shape and thickness of the sample 4. Further, the sample table 9 is X, Y
It is attached to the stage 7, and the X, Y stage 7 is attached to the sample rotating mechanism 8. The X, Y stage 7 can move the incident position of the incident X-ray 3 on the surface of the sample 4, and the sample rotation mechanism 8 can move the incident X-ray 3.
The sample 4 can be rotated with the wire 3 as the axis of rotation.

[Procedure Amendment 5]

[Document name to be amended] Statement

[Name of item to be corrected] 0024

[Correction method] Change

[Correction content]

[0024] Although not shown in the drawings, the rotating mechanism 8, X of the sample stage 9, Y stage 7 and the Z stage is driven by a motor system <br/> control circuit is further controlled by the computer 12.

[Procedure correction 6]

[Document name to be amended] Statement

[Name of item to be corrected] 0025

[Correction method] Change

[Correction content]

The diffracted X-rays 5 diffracted by the sample 4 are X-rays.
It is measured by the line detector 6. In the case of this embodiment, the curved position-sensitive X-ray detector is used, but a linear detector may be used. In this embodiment, the back reflection Laue spots are arranged to be measured, and the measurable diffraction angle 2θ is 10 °.
To 170 °.

[Procedure Amendment 7]

[Document name to be amended] Statement

[Correction target item name] 0056

[Correction method] Change

[Correction content]

[0056] (5) In another embodiment the present invention of the present invention, it may be used X-ray focusing device for focusing the incoming morphism X-ray beam.

[Procedure Amendment 8]

[Document name to be amended] Statement

[Correction target item name] 0063

[Correction method] Change

[Correction content]

(Claim 4) To collect the incident X-ray
Of which deployed X-ray focusing element, there is an effect that high-accuracy measurement data is obtained from the small region of the sample.

Claims (7)

[Claims] 1. A sample stage having a mechanism for holding a sample to be measured and rotating at least around an incident X-ray, an X-ray source for irradiating the sample with white X-rays at a predetermined incident angle, and the sample. An X-ray detector that measures and outputs diffracted X-rays diffracted from the above, and controls each of the above-mentioned parts, and calculates a diffraction angle from the measured value from the X-ray detector to determine the rotation angle of the sample and the diffracted X-ray. An X-ray diffractometer, comprising: a computer for synthesizing an diffraction angle and an X-ray diffraction pattern. 2. The X-ray according to claim 1, wherein the sample stage is provided with a mechanism for rotating around the incident X-ray and a mechanism for moving the incident X-ray in a three-dimensional direction. Diffraction device. 3. The X-ray diffractometer according to claim 1, wherein a position-sensitive detector capable of simultaneously measuring a plurality of diffracted X-rays from a sample is provided as the X-ray detector. 4. The X-ray diffractometer according to claim 1, wherein an X-ray detector having an X-ray condensing element for condensing an incident X-ray beam is provided as the X-ray detector. .. 5. A mechanism for rotating the sample stage, an X-ray source, an X-ray detector, a sample stage around an incident X-ray, and an incident X-ray.
A mechanism for moving in a three-dimensional direction with respect to the X-ray is housed in a vacuum measuring container provided with a vacuum evacuation means, and a mechanism for rotating the sample stage around the incident X-ray or 3 for the incident X-ray. The mechanism for moving in the dimensional direction is configured to be operable from the outside of the vacuum measuring container.
Alternatively, the X-ray diffractometer according to item 4. 6. The computer has a function of storing X-ray diffraction information of a known substance, and an X-ray diffraction pattern calculation function of calculating an X-ray diffraction pattern from the stored X-ray diffraction information.
2. A substance judging function for judging the substance identification of the sample to be measured by comparing the measured X-ray diffraction pattern with the X-ray diffraction pattern obtained by the calculation. X-ray diffractometer. 7. An X-ray diffraction pattern calculation function for calculating an X-ray diffraction pattern from X-ray diffraction information of a sample to be measured, which has been input to the computer in advance, and the measured X-ray diffraction pattern and the calculation result. The X-ray diffractometer according to claim 1, further comprising a crystal orientation analysis function for analyzing a crystal orientation of a sample to be measured by comparing it with the X-ray diffraction pattern.