JPH11304731A - X-ray device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an X-ray device that can freely select a desired X-ray measurement out of a number of types of X-ray measurement, can securely prevents a sample being measured from falling, and further easily install an environmental attachment. SOLUTION: An X-ray device is provided with an X-ray source F for generating X rays, a θ rotary stand 9 for rotating a sample S with a ω axial line passing through the surface of the sample S as a center, an X-ray counter 2 for detecting X rays R2 that are diffracted by the sample S, a 2θ' attachment 15 for supporting the X-ray counter 2, and a 2θ rotary stand 11 for rotating the attachment 15 with the ω axial line as a center. The 2θ' attachment 15 rotates the X-ray counter 2 with the 28' axial line that orthogonally crosses the ω axial line as a center. By appropriately selecting and executing each operation of the θrotary stand 9, the 2θ rotary stand 11, and the 2θ' attachment 15, each kind of X-ray measurement can be selectively executed.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an X-ray apparatus having a structure in which when a sample is irradiated with X-rays, X-rays diffracted by the sample are detected by X-ray detecting means.

[0002]

2. Description of the Related Art Conventionally, there are various types of X-ray apparatuses having various structures and various uses. For example, an X-ray apparatus equipped with a θ-2θ rotary goniometer suitable for analyzing a powder sample, an X-ray apparatus equipped with a 4-axis goniometer suitable for analyzing a single crystal sample such as a silicon wafer, quartz, or the like, There are an in-plane measurement X-ray apparatus that performs measurement by scanning and moving a counter in an in-plane direction parallel to the surface of a sample, that is, a so-called latitude direction, and various other X-ray apparatuses.

Now, considering an X-ray apparatus equipped with a four-axis goniometer, this X-ray apparatus is, for example, as shown in FIG.
X-ray generator 51 including X-ray source F, X-ray counter 52
And a four-axis goniometer 53. The four-axis goniometer 53 includes, for example, a θ rotation table 59, a 2θ rotation table 61, and a 2θ rotation table
A counter arm 62 extending in the outer diameter direction from 1 and supporting the X-ray counter 52, and a counter arm 62 provided on the θ-turntable 59.
(Chi) circle 66 and this χ (chi) circle 66
And a gonio head 58 that supports the sample S.

The θ turntable 59 and the 2θ turntable 61 are coaxially arranged around a vertical axis passing through the surface of the sample S, that is, the θ axis, and are configured to rotate independently. You. The χ (chi) circle 66 is configured to rotate synchronously with the θ-turntable 59 about the θ-axis and to rotate 2θ ′ about the χ-axis perpendicular to the θ-axis.

While the sample S is supported by the gonio head 58, the rotation center O at the intersection of the θ axis and the χ axis is
It is located in. The mounting of the sample S on the gonio head 58 is performed by a known method, for example, using an adhesive or the like. The gonio head 58 rotatably supports the sample S about the central axis ω. This center axis ω rotates about the rotation center O in accordance with the rotation of the χ (chi) circle 66, and FIG. 3 shows a state in which the ω axis and the θ axis coincide with each other.

According to the X-ray apparatus using the four-axis goniometer, the sample S can be set at an arbitrary angle in the three-dimensional space with respect to the incident X-ray R1, so that when the sample S is a single crystal material, The specific diffraction angle specific to the sample S is searched for, and the position of the sample S can be set at that angle position.

Next, an X-ray apparatus equipped with the above-mentioned θ-2θ rotary goniometer is shown in FIG.
X having a structure in which a χ (chi) circle 66 is removed from 9 and the sample S is directly supported by the θ turntable 59
Considered a wire device. In this X-ray apparatus, the θ turntable 59
Rotates the sample S intermittently or continuously at a predetermined angular velocity in a certain direction, so-called θ rotation, and at the same time, the 2θ turntable 61 moves the counter arm 62 in the same direction at twice the angular velocity of θ rotation, thus X The line counter 52 will be rotated.

The X-ray apparatus for in-plane measurement is an X-ray diffraction analysis method using in-plane (in-plane diffraction). This in-plane diffraction is a phenomenon in which when an X-ray R1 is incident on the surface of a sample S at a small incident angle δ, a diffraction line R3 is generated at a small angle with respect to the sample surface as shown in FIG. is there. This is X
When the ray R1 is incident on the sample S at a small incident angle, an X-ray component running parallel to the sample surface appears inside the sample S, which causes diffraction by a crystal plane perpendicular to the sample surface. It is based on the phenomenon of coming out of the surface.

This in-plane diffraction is a method suitable for thin film evaluation, and is very useful for evaluation of a sample having a small film thickness or a sample having an in-plane orientation in relation to a substrate. is there. In order to realize this in-plane measurement, the X-ray counter 52 must be rotated by 2θ for adjusting the optical position, and in order to detect in-plane diffraction lines, the X-ray counter 52 must be rotated in a plane orthogonal to the 2θ rotation plane. The scan rotation must be performed in the direction, that is, the latitude direction 2θ ′.

[0010]

With respect to conventionally known X-ray apparatuses, dedicated X-ray apparatuses have been used for performing various kinds of measurements as described above or other measurements. Therefore, a large amount of expense was required to perform various measurements, and an installation space was required for each dedicated machine, and further, maintenance and inspection work and management required a great deal of labor and labor. .

Particularly, in the liquid crystal device using the four-axis goniometer shown in FIG. 3, since the sample S is rotated by a circle, the sample may drop off during the measurement, or the movement accuracy of the sample, that is, the measurement accuracy may be reduced. There is a problem that large errors are likely to occur. In addition, there is a problem that it is difficult to additionally attach an environmental attachment such as a sample high-temperature device, a gas replacement device, and the like due to the presence of a circle.

The present invention has been made in view of the above problems in the conventional X-ray apparatus, and is intended to freely select and execute a desired X-ray measurement from various types of X-ray measurements. It is an object of the present invention to provide an X-ray apparatus capable of reliably preventing a sample from dropping out during a measurement, and further capable of easily installing an environmental attachment.

[0013]

(1) In order to achieve the above object, an X-ray apparatus according to the present invention comprises an X-ray source for generating X-rays and an ω-axis passing through the surface of a sample. A θ-turntable for rotating the sample, X-ray detection means for detecting X-rays diffracted by the sample, and 2 supporting the X-ray detection means
It has a θ ′ attachment and a 2θ turntable that rotates the 2θ ′ attachment about the ω axis. The 2θ ′ attachment rotates the X-ray detecting means around a 2θ ′ axis orthogonal to the ω axis.

According to this X-ray apparatus, a 2θ ′ attachment is provided on a 2θ turntable, and the 2θ ′ attachment is centered on a 2θ ′ axis orthogonal to the ω axis which is the rotation centerline of the 2θ turntable. Since the X-ray detection means can be rotated, the θ-2θ-based goniometer can be used by appropriately combining the θ rotation of the sample, the 2θ ′ rotation of the attachment and the 2θ ′ rotation of the X-ray detection means as needed. Measurement using a four-axis goniometer, measurement requiring an angle measurement in the latitude direction such as in-plane measurement, and various other X-ray measurements can be performed by one X-ray device.

(2) In the X-ray apparatus having the above structure,
The θ-turntable is 2 independent of the rotation of the sample by the θ-turntable.
It is desirable to configure so that the θ ′ attachment is rotated. By doing so, the degree of freedom of rotation between the θ-turntable and the 2θ-turntable is increased, so that it is possible to cope with more types of X-ray measurements.

(3) In the X-ray apparatus having the above configuration,
A counter arm is provided on the 2θ turntable, the counter arm is rotated by the 2θ turntable about the ω axis, and the 2θ ′ attachment is removably disposed on the counter arm. It is desirable to do. In this way, when the rotation in the latitude direction performed using the 2θ ′ attachment is unnecessary, by removing the 2θ ′ attachment,
The structure of the X-ray optical system can be simplified.

(4) In the X-ray apparatus of (3),
A guide portion for positioning the 2θ ′ attachment may be provided on the counter arm, and the guide portion may be configured to guide the 2θ ′ attachment such that the 2θ ′ axis is orthogonal to the ω axis. In this case, when the 2θ ′ attachment is mounted on the counter arm, the 2θ ′ axis is automatically positioned at a predetermined position intersecting with the ω axis, so that the assembly accuracy of the X-ray optical system is improved, and the X-ray The optical axis accuracy of the optical system is improved.

(5) In the X-ray apparatus having the above configuration,
It is preferable that the 2θ ′ axis is configured to extend in a direction perpendicular to the optical axis of the X-rays captured by the X-ray detection unit. With this configuration, the X-ray detection unit can be accurately rotated and moved in the latitude direction of the sample, that is, in the direction in which the X-ray detection unit rotates around the normal to the sample surface, while maintaining a constant inclination angle with respect to the sample.

[0019]

FIG. 1 shows an embodiment of an X-ray apparatus according to the present invention. The X-ray apparatus includes an X-ray generator 1 including an X-ray source F that generates an X-ray R1 incident on a sample S, an X-ray counter 2 that detects a diffracted X-ray R2 from the sample S, A goniometer 3 for measuring the position of the X-ray counter 2. The X-ray source F is fixedly arranged, and can be configured to include, for example, a filament that emits thermoelectrons when energized, and a target with which the thermoelectrons collide at a high speed. In this case, X-rays are generated from the target hit by the thermoelectrons.

Between the X-ray source F and the sample S, a divergence regulating slit for regulating the divergence of the X-ray R1 so that the X-ray R1 diverging from the X-ray source F enters the sample S; An incident side optical unit 4 including various X-ray optical elements such as a monochromator for monochromatic continuous X-rays is provided. Further, between the sample S and the X-ray counter 2, a scattered-ray regulating slit for preventing unnecessary X-rays such as scattered X-rays from being taken into the X-ray counter 2, and a focusing position of the X-ray R <b> 2. A light receiving side optical unit 6 including various X-ray optical elements such as a light receiving slit and the like is disposed. The X-ray counter 2 is, for example, an SC (Scintillatio).
n Counter).

The goniometer 3 is installed on a gantry 7 and supports a sample S. The goniometer 3 is provided around a goniometer head 8, a θ turntable 9 supporting the goniometer head 8, and the θ turntable 9. It is configured to include a 2θ turntable 11 and a counter arm 12 extending from the 2θ turntable 11 in the outer diameter direction. turntable 9 is configured to be rotatable about a vertical ω axis passing through the surface of the sample S. The 2θ turntable 11 is also configured to be able to rotate about the ω axis.

As shown in FIG. 2, the θ-rotation table 9 is driven by the θ-rotation drive device 13 and rotates intermittently or continuously at a predetermined angular velocity about the ω-axis. Also, 2θ
The turntable 11 is driven by the 2θ rotation drive device 14 and rotates about the ω axis, and turns the X-ray counter 2 on the sample S
Rotate against In this manner, the θ rotation table 9 and the 2θ rotation table 11 are arranged coaxially with each other, and their rotation is controlled independently of each other. These θ rotation driving devices 13 and 2θ
The rotary drive 14 can be configured using any drive,
For example, it can be configured using a power transmission mechanism including a worm and a worm wheel.

On the counter arm 12, a 2θ 'attachment 15 is detachably mounted. In the present embodiment, a guide portion 29 is formed on the counter arm 12, and in a state where the guide portion 29 is positioned by the guide portion 29, the 2θ ′ attachment 15 is attached to the counter arm 12.
Fixed on top.

The 2θ ′ attachment 15 is provided on the support member 2.
8 and an attachment arm 16 that can rotate about the 2θ ′ axis, and a 2θ ′ rotation drive device 17 that rotationally drives the attachment arm 16. The 2θ ′ rotation drive device 17 includes, for example, a drive motor 18 including a pulse motor, and a worm 19 that is driven and rotated by the drive motor 18.
And the worm wheel 21 meshing with the worm 19
It is comprised including. Of course, it can be configured using any other power transmission mechanism. In addition, 2
The θ ′ rotation drive device 17 includes the θ rotation drive devices 13 and 2θ
The operation is controlled independently of the rotation drive device 14.

With the above configuration, the X-ray counter 2 supported on the counter arm 12 via the attachment arm 16 rotates around the ω axis in accordance with the rotation of the 2θ turntable 11 driven by the 2θ rotation driving device 14. It is configured to rotate and further driven by a 2θ ′ rotation drive device 17 to rotate about the 2θ ′ axis.

The sample S is supported, for example, by a gonio head 8 and is located at the intersection O between the ω axis and the 2θ ′ axis, and rotates relative to the X-ray source F about the ω axis as indicated by the symbol θ. I do. On the other hand, the X-ray counter 2
As shown by, the sample rotates relative to the sample S about the ω axis. The X-ray counter 2 rotates relative to the sample S about the 2θ ′ axis as indicated by reference numeral 2θ ′. The sample S can be supported by any support structure other than the gonio head.

Theta rotation drive device 13, 2θ rotation drive device 1
4 and 2θ ′ rotation driving device 17
0 controls their operation. The X-ray measurement control device 20 includes a CPU 22 and a memory 23 attached thereto. The memory 23 stores a program that controls the overall control of the X-ray diffraction measurement. CP
The output port of U22 is connected to a CRT (Cathode Ray Tube) display 24 as a display device in addition to the θ rotation drive device 13, 2θ rotation drive device 14, and 2θ ′ rotation drive device 17.

On the other hand, an X-ray intensity calculation circuit 26 is connected to an input port of the CPU 22. The X-ray intensity calculation circuit 26 is connected to the output terminal of the X-ray counter 2 and calculates the intensity of the X-ray R2 captured by the X-ray counter 2 based on the output signal of the X-ray counter 2. Then, the X-ray intensity calculated by the X-ray intensity calculation circuit 26 is transmitted to the CPU 22 as an electric signal. The input port of the CPU 22 is connected to an input device 25 such as a keyboard and a mouse-type input device in addition to the X-ray intensity calculation circuit 26.

Since the X-ray apparatus of this embodiment is configured as described above, the following various rotations, ie, when the gonio head 8 is used, the vertical and horizontal directions of the sample S performed by the gonio head 8 Rotation of the sample S performed by the θ rotation table 9, 2θ rotation of the 2θ ′ attachment 15 performed by the 2θ rotation table 11, and 2θ ′ rotation of the X-ray counter 2 performed by the 2θ ′ attachment 15. By selecting and executing various rotations, the X-ray diffraction measurement of θ-2θ method, X-ray diffraction measurement equivalent to 4-axis goniometer, X-ray diffraction measurement of in-plane diffraction line, and all other types X-ray measurements can be made as desired.

(1) Measurement Example 1 For example, when performing X-ray diffraction measurement of θ-2θ method on a powder sample, first, the 2θ ′ attachment 15 is used to set the position of 2θ ′ = 0 °, that is, the sample 2 The X-ray counter 2 is set at a position where the incident X-rays R1 incident thereon and the diffracted X-rays R2 diffracted by the sample S enter the same horizontal plane. In this state, the sample S is intermittently or continuously rotated by θ at a constant angular velocity in a fixed direction by the θ turntable 9, and at the same time, the X-ray counter 2 is rotated by θ by the 2θ turntable 11.
Rotate 2θ in the same direction at twice the angular velocity of rotation.

When the Bragg diffraction condition is satisfied between the X-ray R1 incident on the sample S and the crystal lattice plane of the sample S while the sample S rotates by θ, the X-ray is diffracted by the sample S, The diffraction line is detected by the X-ray counter 2, and the X-ray intensity is calculated by the X-ray intensity calculation circuit 26.
The line intensity value is stored in a predetermined storage location of the memory 23 by the processing of the CPU 22. Thus, the relationship between the angular position of the X-ray counter 2, that is, the diffraction angle 2θ, and the diffracted X-ray intensity at that angular position is measured.

In this embodiment, the 2θ ′ attachment 15 is detachably attached to the counter arm 12. Therefore, the 2θ ′ attachment 15 is detached from the counter arm 12 and the X-ray counter
Is mounted on the counter arm 12, the 2θ turntable 1
By rotating the counter arm 12 by 2θ by 1, the measurement can be performed by an X-ray optical system similar to a normal θ-2θ goniometer. In this case, since the X-ray optical system becomes simple, optical adjustment of the optical system can be easily performed.

In the present embodiment, the counter arm 12
A guide portion 29 is provided at a predetermined position of the guide portion 2.
When the 2θ ′ attachment 15 is attached along 9, the 2θ ′ axis is automatically orthogonal to the ω axis. Therefore, as described above, the 2θ ′ attachment 1
When the 5 is attached to and detached from the counter arm 12, the 2θ 'axis can be stably positioned at a constant position with respect to the ω axis by simply operating the 2θ' attachment 15 along the guide portion 29.

(2) Measurement Example 2 Next, a case where a measurement equivalent to the X-ray diffraction measurement using the four-axis goniometer described with reference to FIG. 3 will be described. In FIG. 3, the sample S
It rotates about the axis, rotates about the χ axis by the circle 66, and further tilts and moves by the gonio head 58. The X-ray counter 52 is rotated around the θ axis by the 2θ rotation table 61. By performing these various rotations as desired, a diffraction line generated in the single crystal sample S can be captured by the X-ray counter 52.

In order to perform an equivalent X-ray measurement using the X-ray apparatus of the present embodiment shown in FIG. 1, the sample S is rotated around the ω axis by the θ-turntable 9 and the sample S is tilted by the gonio head 8. Moving, rotating the X-ray counter 2 around the ω-axis by the 2θ turntable 11, and rotating the X-ray counter 2 around the 2θ′-axis by the 2θ ′ attachment 15. By selecting and executing the rotation, the measurement equivalent to the four-axis goniometer shown in FIG. 3 can be performed.

Incidentally, in the conventional X-ray apparatus using a four-axis goniometer shown in FIG.
Due to the existence of the sample 6, it was difficult to mount an environmental attachment around the sample S, such as a sample high-temperature device for adjusting the temperature of the sample, a gas replacement device for adjusting the gas atmosphere around the sample, and the like. In contrast, FIG.
In the present embodiment shown in FIG. 7, since no obstructive member such as a circle is present around the sample S, the environmental attachment can be easily attached.

(3) Measurement Example 3 Next, the case where the in-plane diffraction measurement shown in FIG. 4 is performed will be described. In this case, the flatness of the sample S with respect to the incident X-ray R1 is adjusted by the gonio head 8, and the X-ray incident angle is adjusted to the minute angle δ by rotating the sample S around the ω axis by the θ-turntable 9. Then, the X-ray counter 2 is rotated around the ω-axis by the 2θ turntable 11 to set the position to the minute angular position δ at which the in-plane diffraction line can be detected. By rotating the sample S in the latitudinal direction by rotating it by 2θ about the axis, in-plane diffraction lines generated in the sample S are detected.

As described above, the present invention has been described with reference to the preferred embodiments. However, the present invention is not limited to the embodiments, and can be variously modified within the scope of the invention described in the claims. In the above description, three types of X-ray measurement that can be performed by the X-ray apparatus shown in FIG. 1 have been described.
Tilt rotation of the sample S in the vertical and horizontal directions performed by the gonio head 8, θ rotation of the sample S performed by the θ rotation table 9, and 2 performed by the 2θ rotation table
2θ rotation of θ ′ attachment 15 and 2θ ′ of X-ray counter 2 performed by 2θ ′ attachment 15
By arbitrarily selecting and executing various rotations of rotation,
Any X-ray diffraction measurement other than the above three types can be performed.

[0039]

According to the X-ray apparatus of the present invention, a 2θ 'attachment is provided on a 2θ turntable, and
The θ ′ attachment can rotate the X-ray detection means around a 2θ ′ axis orthogonal to the ω axis which is the rotation centerline of the 2θ turntable, so that the θ rotation of the sample, 2θ ′
By appropriately combining the 2θ rotation of the attachment and the 2θ ′ rotation of the X-ray detection means as needed,
Measurement using a 2θ-based goniometer, measurement using a 4-axis goniometer, measurement that requires angle measurement in the latitude direction such as in-plane measurement, and various other X-ray measurements
Can be performed by two X-ray devices. This allows
The cost can be saved, the installation place of the X-ray apparatus can be reduced, and the labor for maintenance and inspection work and management can be reduced.

[0040]

[Brief description of the drawings]

FIG. 1 is a perspective view showing an embodiment of an X-ray apparatus according to the present invention.

FIG. 2 is a plan view of the X-ray apparatus of FIG. 1 and a diagram showing a control system for the X-ray apparatus.

FIG. 3 is a perspective view showing an example of a conventional X-ray apparatus, particularly an X-ray apparatus using a four-axis goniometer.

FIG. 4 is a diagram schematically showing an in-plane diffraction measurement method which is an example of the X-ray diffraction measurement method.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 X-ray generator 2 X-ray counter 3 Goniometer 4 Incident-side optical unit 6 Receiving-side optical unit 7 Mounting stand 8 Goniotic head 9 θ rotation table 11 2θ rotation table 12 Counter arm 13 θ rotation driving device 14 2θ rotation driving device 15 2θ 'attachment Reference Signs List 16 attachment arm 18 drive motor 19 worm 20 X-ray measurement control device 21 worm wheel 28 support member 29 guide part R1, R2 X-ray S sample

Claims (5)

[Claims] An X-ray source for generating X-rays; a θ-turntable for rotating the sample around an ω-axis passing through the surface of the sample; X-ray detection means for detecting X-rays diffracted by the sample; A 2θ ′ attachment for supporting the X-ray detecting means, and a 2θ turntable for rotating the 2θ ′ attachment about the ω axis, wherein the 2θ ′ attachment is 2θ ′ orthogonal to the ω axis
An X-ray apparatus, wherein the X-ray detection means is rotated about an axis. 2. The X-ray apparatus according to claim 1, wherein the 2θ turntable rotates the 2θ ′ attachment independently of rotation of the sample by the θ turntable. 3. The method according to claim 1, wherein
An X-ray apparatus, wherein the θ-turntable rotates a counter arm about the ω axis, and the 2θ ′ attachment is detachably mounted on the counter arm. 4. The counter arm according to claim 3, wherein the counter arm has a guide portion for positioning a 2θ ′ attachment, and the guide portion adjusts the 2θ ′ attachment so that the 2θ ′ axis is orthogonal to the ω axis. An X-ray apparatus characterized by guiding. 5. The method according to claim 1, wherein the 2θ ′ axis is orthogonal to the ω axis, and
An X-ray apparatus characterized by being coincident with a plane passing through an optical axis of a line.