JP3462910B2 - X-ray incident angle setting method and mechanism for grazing incidence X-ray apparatus - Google Patents

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a microscopic angle for easily and accurately setting an incident angle when an X-ray is incident at a microscopic angle on a sample having a horizontal measuring surface such as a liquid sample. The present invention relates to an X-ray incident angle setting method for an incident X-ray device and its mechanism.

[0002]

2. Description of the Related Art As a conventional X-ray incidence angle setting method and mechanism for a small-angle incidence X-ray apparatus, those shown in FIGS. 6 and 7 are known. The small-angle incidence X-ray apparatus 1 shown in FIG. 6 has a center O of the rotary shaft 3 of an apparatus body 2 such as a sample horizontal goniometer.
A sample 4 is horizontally provided on the outer peripheral surface of the apparatus main body 2, and a central axis C1 including the surface of the sample 4 and intersecting the center O of the rotating shaft 3
An X-ray incidence arm 5 is provided along the line. An X-ray source 6 for generating X-rays is attached to the X-ray entrance arm 5, and the divergence angle of the X-rays emitted from the X-ray source 6 is set near the center to determine the area of the X-rays that hit the sample. A divergence slit 7 is provided to limit

An X-ray detecting arm 8 is provided on the outer peripheral surface of the apparatus main body 2 on the opposite side of the X-ray incident arm 5 along a central axis C2 intersecting with the center O of the rotating shaft 3.
The line detection arm 8 is provided with a scattering slit 9, a solar slit 10, a light receiving slit 11, and a detector 12 from the inside. Reference numeral 13 is a pedestal on which the small-angle incidence X-ray apparatus 1 is placed, and 14 is an adjusting screw for adjusting the horizontal position of the sample.

In this small-angle incidence X-ray apparatus 1, the X-rays emitted from the X-ray source 6 of the X-ray incidence arm 5 pass through a divergence slit 7 and are reflected on the surface of a horizontal sample 4 fixed to a rotating shaft 3. The diffracted X-rays emitted from the sample 4 are detected by the detector 12 via the scattering slit 9, the solar slit 10 and the light-receiving slit 11 of the X-ray detecting arm 8. As the X-ray incident angle setting method in this apparatus, the X-ray incident arm 5 is rotated around the rotation axis 3 at a rotation angle θs to change the incident angle to the sample 4 and at the same time, the X-ray detection arm is rotated. The diffracted X-ray is measured by rotating 8 around the central axis 3 at a rotation angle θd.

In the conventional small-angle incidence X-ray device 21 shown in FIG. 7, the X-ray source 6 of the device main body 2 shown in FIG. 6 is separated from the tip of the X-ray incidence arm 5, and the X-ray incidence arm is separated. 5 is installed on the base 22 near the tip surface of the device 5, and the device main body 2
The pedestal 23 is provided with three adjusting screws 24 for adjusting the height and the inclination angle of the apparatus body 2.

The X-ray incident angle setting method for this apparatus is as follows:
The tilt of the pedestal 23 is adjusted by adjusting the height of the adjusting screw 24 provided on the left side or the right side of the pedestal 23 in FIG. The incident angle of the X-ray that is incident on the sample 4 from the source 6 via the X-ray incidence arm 5 is set. Then X-ray source 6
When the X-ray is diverged from the X-ray, the X-ray is incident on the sample 4 through the divergence slit 7, and the diffracted X-ray from the sample 4 passes through the scattering slit 9, the solar slit 10 and the light receiving slit 11 of the X-ray detecting arm 8. After that, it is detected by the detector 12.

[0007]

However, in the method for setting the X-ray incident angle in the conventional small-angle incidence X-ray apparatuses 1 and 21 described above, in the one shown in FIG. 6, the incident angle θs from the X-ray source 6 is changed. For this purpose, the X-ray source 6 needs to be provided integrally with the X-ray incidence arm 5 and rotated around the sample 4, so the size of the apparatus becomes large, and the X-ray source 6 is used for small-angle incidence X-rays. Since the apparatus occupies the X-ray source 6, there is a problem that the X-ray extraction ports formed at four horizontal positions cannot be used for other X-ray apparatuses.

Further, in the structure shown in FIG. 7, since the X-ray source 6 and the X-ray incidence arm 5 are separated, the positional relationship between the X-ray source 6 and the sample 4 is not fixed and the X-ray source 25 The irradiation position of the X-rays emitted from the sample 4 on the sample 4 is not constant, and the X-ray optical system must be readjusted every time the X-ray incident angle is changed, which makes the operation very complicated and troublesome. There was a problem.

The present invention has been made to solve the above-mentioned problems, and it is possible to easily adjust the minute incident angle of X-rays emitted from an X-ray source on a horizontal sample with a simple structure. Small angle incidence X, which allows the incident X-rays on the horizontal sample to be always applied to the same irradiation position on the sample.
It is an object of the present invention to provide an X-ray incident angle setting method for an X-ray device and its mechanism.

[0010]

In order to solve the above-mentioned problems, the invention according to claim 1 makes an X-ray emitted from an X-ray source incident on a sample surface provided in the center of the apparatus body at a minute angle. In the method for setting an X-ray incident angle of a small-angle incident X-ray device, the small-angle incident X-ray device is placed on an inclined table for setting a minute incident angle of X-rays, and the inclined table is always used for the X-ray source. It is characterized in that it is tilted about a rotation center axis including

According to a second aspect of the present invention, a sample irradiated with X-rays emitted from an X-ray source and a sample holder for holding the sample rotate a rotary shaft fixed at one end thereof to horizontally rotate the sample. An apparatus main body for holding the device, an X-ray incidence arm provided between the apparatus main body and the X-ray source so that the angle can be adjusted according to the X-ray extraction angle, and the apparatus. An X-ray incidence angle setting mechanism of a small-angle incidence X-ray device, comprising an X-ray detection arm that is rotatably provided around a main body and detects an X-ray diffracted from the sample.
With the line source is provided at a distance from the tip of the X-ray incidence arm, a support member to which the X-ray incident angle setting mechanism is provided in the vicinity of the X-ray source, in the upper part of the support member, prior to
The locking member that rotates around the rotation center axis including the X-ray source, the tilting table having one end side fixed to the lower end portion of the locking member and mounting the small-angle incidence X-ray device, and the tilting table. The tilting angle setting screw for adjusting the tilting angle of the tilting table is provided at the end opposite to the fixed end of the locking member.

According to a third aspect of the present invention, the locking portion of the locking member is formed in a wedge shape, and the wedge-shaped locking portion is formed on the top portion of the support member so as to coincide with the rotation center axis. It is characterized by being locked in the groove.

According to a fourth aspect of the present invention, a screw whose height position can be adjusted is provided at the locking portion of the locking member, and the locking member of the screw is provided so that the locking portion of the screw coincides with the rotation center axis. It is characterized by being locked in a recess formed in the top.

According to a fifth aspect of the present invention, the locking portion of the locking member is formed in a spherical shape, and the spherical locking portion of the supporting member is rotated so that the rotation center axis and the rotation center coincide with each other. It is characterized by being locked at the top.

According to a sixth aspect of the present invention, a tilt angle fixing screw for fixing the tilt angle of the tilt table set by the tilt angle setting screw is provided on the fixed end side of the locking member of the tilt table. The feature is that it is provided.

According to a seventh aspect of the present invention, the lower end portion of the locking member is detachably fixed to one end of the tilt base, and the base end portion of the support member is detachably fixed to the base base. It is characterized by that.

The invention according to claim 8 is characterized in that the tip of the tilt angle setting screw is provided so as to be horizontally movable on the base according to the rotation of the tilt base.

[0018]

According to the present invention, since the rotation center axis of the locking portion of the locking member fixed to one end of the tilt table is coincident with the X-ray source, it is possible to rotate the tilt angle setting screw of the tilt table. The tilt angle of the tilt table changes about the rotation center axis, and the X-ray extraction angle from the X-ray source changes, which changes the X-ray incident angle on the horizontal sample. Further, since the center axis of rotation of the tilt table always rotates about the X-ray source as the center of rotation, the incident X-ray flux is always irradiated on the same irradiation position on the horizontal sample.

[0019]

The present invention will be described in detail with reference to the drawings.
1 to 4 show an X-ray incidence angle setting mechanism of a small-angle incidence X-ray apparatus according to an embodiment of the present invention, which is designated by reference numeral 31.
Is an X-ray incident angle setting mechanism (hereinafter simply referred to as "X-ray incident angle setting mechanism") of the small angle incident X-ray apparatus. The X-ray incidence angle setting mechanism 31 is provided with a pedestal 33 of a small-angle incidence X-ray device 32.
Is mounted on the tilt table 34, and the tilt table 34 is further mounted on the base table 35. On the base table 35, the side of the small-angle incidence X-ray device 32 mounted on the tilt table 34 ( An X-ray generator 36 is provided on the right side in FIG. 1, and two support members 37 are provided on both sides of the X-ray generator 36 in parallel with the center line O of the rotation axis of the small-angle incidence X-ray device 32. A locking member 38 that rotates the tilt table 34 about the upper surface of the support member 37 is provided between the support member 37 and the tilt table 34.

Device main body 32 of small-angle incidence X-ray device 32
a, a rotary shaft 41 is provided at the center of, for example, a vertical goniometer, and the rotary shaft 41 is provided at the protruding end of the rotary shaft 41.
A sample holder 41a that rotates together with the sample holder 41a is provided.
The protruding end of the rotary shaft 41 has a lower half formed in a semicircular cross section by notching the upper half horizontally, and a sample 42 for X-ray analysis on the horizontal portion of the rotary shaft 41 having the semicircular cross section. Is attached to the sample holder 41a. Then, the rotation shaft 41 is rotated to hold the sample holder 41a in a horizontal state, and in particular, when the sample 42 is a liquid material, the sample is injected into the sample holder 41a so that the horizontal surface of the sample can be maintained. Is formed. Further, on the outer peripheral surface of the small angle incidence X-ray device 32, an X-ray incidence arm 43 for guiding the X-rays emitted from the X-ray generator 36 to the sample 42,
X-ray detection arm 4 for detecting diffracted X-rays from the sample 42
And 4 are rotatably provided about the rotation shaft 41.

The X-ray incidence arm 43 has a divergence slit 45 for limiting the X-ray area by irradiating the sample by limiting the horizontal divergence angle of the X-ray, and a single crystal plane having a single crystal. For example, a monochromator 46 for monochromaticizing the X-ray from the sample using the surface of germanium is provided. The monochromator 46 can remove not only the background but also the κβ rays that cannot be completely removed by the κβ filter method. In addition, the X-ray detection arm 44 has a scattering slit 47 for removing scattered X-rays from a place other than the sample such as air scattering, and limits only the vertical divergence of the diffracted X-rays so that only the central part of the Debye ring is formed. A solar slit 48 for taking out, a light receiving slit 49 for adjusting the resolution of diffracted X-rays, a detector 50 for detecting X-rays, and the like are provided.

In the X-ray generator 36, an X-ray source 53 is composed of an electron gun 51 that emits thermoelectrons upward from a filament and a drum-shaped target 52 that receives the thermoelectrons while rotating at high speed. The X-ray source 53 is covered by the tube shield 54. The tube shield 54 has windows (not shown) formed on four horizontal surfaces, and X-rays are radiated to the surroundings from the windows.

In the pedestal 33, one is provided at the center of the X-ray detection arm 44 side (left side in FIG. 1) and the X-ray incidence arm 43 is provided.
Two position adjusting screws 33a on both sides of the side (right side in FIG. 1)
Are provided, and the height and horizontal position of the surface of the sample 42 are adjusted by adjusting these position adjusting screws 33a. Further, the tilt table 34 has an X-ray detection arm 44.
One tilt angle setting screw 34a is attached to the center of the side, and two tilt angle fixing screws 34b are attached to both side parts on the X-ray incidence arm 43 side. By adjusting the tilt angle fixing screw 34b, the tilt angle of the tilt table 34 with respect to the X-ray source 53 is adjusted and held. Further, the tip ends of the tilt angle setting screw 34a and the tilt angle fixing screw 34b are, for example, as shown in FIG.
5 is supported inside a one-way V groove 35b formed on the upper surface of the screw pedestal 35a fixed on the tilt base 3a.
It is possible to move horizontally according to the inclination angle of 4. A ball screw may be attached to the inclined table 34 instead of the V groove 35b.

The supporting member 37 is formed in a cylindrical shape, and the base end portion 37a is detachably fixed to the base 35 with bolts or the like.
Further, a V groove 37b is formed on the upper surface in parallel with the center line O of the rotation axis of the small angle incidence X-ray device 32. A locking member 38 is attached between the support member 37 and the inclined table 34. The upper locking portion 38a of the locking member 38 is formed in a wedge shape, and the wedge-shaped locking portion 38a is the supporting member 37.
Is locked in the V groove 37b. The rotation center axis YY formed by the V groove 37b of the support member 37 and the locking portion 38a of the locking member 38 provided on both sides of the X-ray source is the X-ray source divergent X-ray source. It is provided to match the position. Further, the lower end portion 38b of the locking member 38 is provided on the inclined table 3
4 is detachably fixed to one end of the screw 4 by the screw 55, whereby the tilt table 34 is rotatable about the rotation center axis Y-Y.

Next, the X-ray incident angle setting method of this embodiment will be described.

First, as shown in FIG. 2, a pedestal in which an inclined table 34 is placed on a base 35 to which an X-ray generator 53 is attached, and a small angle incident X-ray apparatus 32 is attached to the upper portion of the inclined table 34. Place 33. X-ray generator 53
A pair of support members 37 are provided on both sides of the
The engaging portion 38a of the engaging member 38 having one end of the inclined table 34 fixed is engaged with the V groove 37b formed at the top of the.

In this state, first, the rotary shaft 41 of the small-angle incidence X-ray device 32 is rotated to hold the sample 42 in the sample holder 41a in a horizontal state, and at the same time, the position adjusting screw 33a of the pedestal 33 and the tilting table 34 are used. Inclination angle setting screw 34
By adjusting the height position of a, the tip of the X-ray incidence arm 43 of the small-angle incidence X-ray device 32 is radiated from the X-ray source 53 to emit X.
Align with the incident position of the line. Note that the tilt angle fixing screw 34 b of the tilt table 34 is floated from the base 35 so that the tilt table 34 can be fixed to the tilt angle setting screw 34 a and the locking member 38.
It is supported in a horizontal state by the front end portion 38a of the.

Next, turn the tilt angle setting screw 34a to
The tilt table 3 on the side provided with the tilt angle setting screw 34a
4 is moved up and down, the tilting table 34 is locked by the locking member 3
The rotation center axis Y-Y formed by the locking portion 38a of No. 8 and the V groove 37b of the support member 37 is inclined. In this embodiment, the rotation center axis Y-Y of the locking member 38 coincides with the X-ray source 53, and by changing the tilt angle of the tilt table 35, the X-ray extraction angle from the X-ray source 53 changes. Therefore, the incident angle on the sample 42 changes.

For example, as shown in FIG. 4, the position of the sample 42 is changed from the position (a) to the position (b) by rotating the tilt table 34.
When the position changes to, the extraction angle of the X-rays from the X-ray source 53 changes from the state of (a) to the state of (b),
As a result, the minute incident angle of X-rays on the horizontal surface of the sample 42 changes from α1 to α2. Further, since the sample 42 has the X-ray source 53 as the center of rotation, the incident X-ray flux always enters the same irradiation position on the surface of the sample 42, for example, the center of the sample surface, even if the sample 42 rotates. In this example,
The incident angle is changed within a minute angle range of 0 to 3 °.

The diffracted X-ray from the surface of the sample 42 is
A scattering slit 47 provided on the X-ray detection arm 44,
Detector 5 through solar slit 48 and light receiving slit 49
Detected at 0. Further, by rotating the X-ray detection arm 44 around the center line O of the rotary shaft 41 of the small-angle incidence X-ray device, 2θ of the diffracted X-ray from the sample can be measured.

As described above, according to the X-ray incident angle setting mechanism 31 of this embodiment, it is only necessary to adjust the tilt angle setting screw 34a and rotate the tilt base 34 about the rotation center axis Y--Y. The small incident angle of X-rays on the sample 42 can be set easily, quickly and surely.

After the small angle of incidence of X-rays on the sample 42 is set, the tilt angle fixing screw 34b of the tilt table 34 is set.
The tilting member 34 is turned on and the tilting base 34 is supported on the base 35 by the tilting angle fixing screw 34b, so that the locking member 38 is locked.
You may make it remove from 4. As a result, the tilting table 34 includes the tilt angle setting screw 34a and the tilt angle fixing screw 3a.
With 4b, a predetermined inclination angle is held, and a predetermined X-ray incident angle is obtained. Further, by removing the support members 37 on both sides of the X-ray generator 53 from the base 35, it becomes possible to use X-rays diverging from both sides of the X-ray source 52, and the effective use of the X-ray generator 53 can be achieved. In addition, the maintenance can be facilitated.

FIG. 5 shows a modification of the wedge-shaped tip and the V-shaped groove which constitute the rotating mechanism for rotating the tilting table 34 of the above-described embodiment about the rotation center axis Y--Y, and the locking member 38.
On the horizontal plate at the upper end of the
The tip of the screw 61 is rotatably locked in a recess 62 formed in the upper surface of the support member 37. In addition to this, the tip end portion of the locking member 38 is formed into a spherical shape, and this spherical end portion is rotated in conformity with the rotation center axis YY, or an axis having the rotation center axis YY as the rotation center. It may be configured with a bearing and the like. Further, as shown in FIG. 5, the connection between the locking member 38 and the inclined base 34 may be achieved by superposing the lower end portion 38b of the locking member 38 on the lower surface of one end of the inclined base 34 and connecting them with a bolt or the like. Alternatively, the tilting base 34 and the locking member 38 may be integrally formed.

In the above embodiment, the support members are provided on both sides of the X-ray generator, but they may be provided on either side, or a tube shield may be used as the support member instead of the support member. You may Further, by controlling the driving of the tilt angle setting screw by a driving source such as a motor, it is possible to change the small angle incidence of X-rays at a constant angular velocity.

In the above embodiment, the X-ray incidence arm is rotatably attached integrally to the outer peripheral surface of the apparatus body.
Alternatively, the X-ray incidence arm may be provided separately from the apparatus main body, a dedicated tilting table may be provided on the base, and the X-ray entrance arm may be independently supported on the tilting table. In this case, a tilt angle setting screw and a tilt angle fixing screw are attached to the tilt table similarly to the tilt table on which the sample horizontal goniometer is mounted, and these are adjusted to adjust the incident X-ray irradiation position on the sample. It is desirable to adjust
Further, in the above-mentioned embodiment, an example using the rotating anticathode type as the X-ray generator is given.
Of course, a line tube may be used.

Furthermore, in the above-mentioned embodiments, the present invention is used for measuring diffracted X-rays from a sample. However, the present invention is not limited to this, and measurement of scattered X-rays, measurement of fluorescent X-rays, measurement of photoelectrons. Of course, it can be applied to the above. When measuring photoelectrons, the device must be placed in a vacuum chamber.

[0037]

As described above, according to the method of the present invention, the extraction angle of X-rays emitted from the X-ray source is changed by changing the inclination of the tilting table with the X-ray source as the rotation center axis. This makes it possible to change the angle of incidence of small-angle incident X-rays on a horizontally installed sample, and even if the angle of incidence is changed, the X-ray optical system will not be displaced and the incident X-rays It is possible to irradiate the same position. Therefore, it is not necessary to readjust the X-ray optical system every time the incident angle is changed, and the sample can be analyzed easily, quickly and accurately.

According to the mechanism of the present invention, the tilt angle of the tilt table is adjusted by rotating the tilt angle setting screw.
The minute incident angle on the sample can be easily changed by changing the extraction angle of the X-ray from the X-ray source.

After the tilt angle of the tilt table is set, the tilt angle of the tilt table can be held by the tilt angle setting screw and the tilt angle fixing screw by adjusting the tilt angle fixing screw. .

Further, by removing the locking member and the support member, there are no obstacles around the X-ray source, the X-ray source can be used in multiple ways, and the maintenance is easy.

[Brief description of drawings]

FIG. 1 is a diagram illustrating an X of a small-angle incidence X-ray device according to an embodiment of the present invention.
It is the whole incident angle setting mechanism perspective view.

FIG. 2 is a front view of FIG.

FIG. 3 is an explanatory diagram illustrating a state in which the tip ends of the tilt angle setting screw and the tilt angle fixing screw of FIG. 1 are provided so as to be horizontally movable inside the groove of the pedestal.

FIG. 4 shows how the X-ray incidence angle setting mechanism of FIG. 1 is used to incline the tilting table to change the extraction angle of X-rays from the X-ray source, thereby changing the X-ray incidence angle to the sample. It is an explanatory view explaining.

FIG. 5 is an explanatory view illustrating a modified example of the rotation center shaft configured by the support member and the locking member of the present invention.

FIG. 6 is a front view of a small-angle incidence X-ray apparatus in which an X-ray source is integrally provided on a conventional X-ray incidence arm.

FIG. 7: Small angle incidence X in which a conventional X-ray source is provided separately
It is a front view of a line device.

[Explanation of symbols]

31 X-ray incidence angle setting mechanism for small-angle incidence X-ray device 32 Micro incidence X-ray equipment 32a device body 33 pedestal 34 Slope 34a Incident angle setting screw 34b Incident angle fixing screw 35 base 36 X-ray generator 37 Support member 37b V groove, recess, 38 Locking member 38a One end of locking member (wedge, screw, spherical end) 38b The other end of the locking member 41 rotation axis 41a sample holder 42 samples 43 X-ray incidence arm 44 X-ray detection arm 53 X-ray source

Claims (8)

(57) [Claims] 1. A method for setting an X-ray incidence angle of a small-angle incidence X-ray apparatus, in which X-rays emitted from an X-ray source are incident on a horizontal sample surface provided in the center of the apparatus body at a minute angle. The incident X-ray device is mounted on an inclined table for setting a minute incident angle of X-rays, and this inclined table is always rotated and inclined about a rotation center axis including the X-ray source. An X-ray incident angle setting method for an X-ray device. 2. A sample irradiated with X-rays emitted from an X-ray source, and an apparatus main body for horizontally holding the sample by rotating a rotary shaft having a sample holder holding the sample fixed at one end. , An X-ray incidence arm that is provided between the apparatus main body and the X-ray source so that the angle can be adjusted according to the extraction angle of X-rays, and can guide the X-rays to the sample. an X-ray incidence angle setting mechanism provided by grazing incidence X-ray apparatus having an X-ray detection arm for detecting the diffracted X-rays from the sample, the X-ray source for the X-ray incidence A support member that is provided apart from the tip of the arm, and the X-ray incident angle setting mechanism is provided in the vicinity of the X-ray source , and above the support member during rotation including the X-ray source.
A locking member that rotates around the mandrel, a tilt table that has one end side fixed to the lower end of the locking member and that mounts the small-angle incidence X-ray device, and a fixing of the locking member of the tilt table. An X-ray incidence angle setting mechanism for a small-angle incidence X-ray apparatus, comprising an inclination angle setting screw for adjusting the inclination angle of the tilt table at the end opposite to the end. 3. The locking portion of the locking member is formed in a wedge shape, and the wedge-shaped locking portion is locked in a V groove formed on the top of the support member so as to coincide with the rotation center axis. The X-ray incidence angle setting mechanism of the small-angle incidence X-ray device according to claim 2. 4. A screw whose height position can be adjusted is provided at the locking portion of the locking member, and a recess formed at the top of the support member so that the locking portion of the screw coincides with the rotation center axis. The X-ray incidence angle setting mechanism of the small-angle incidence X-ray apparatus according to claim 2, characterized in that 5. The locking portion of the locking member is formed in a spherical shape, and the spherical locking portion is locked on the top of the support member so as to rotate with the rotation center axis coincident with the rotation center. The X-ray incidence angle setting mechanism of the small-angle incidence X-ray device according to claim 2. 6. A tilt angle fixing screw for fixing the tilt angle of the tilt table set by the tilt angle setting screw is provided on the fixed end side of the locking member of the tilt table. The small angle incident X according to any one of claims 2 to 5.
X-ray incident angle setting mechanism for X-ray equipment. 7. The lower end portion of the locking member is detachably fixed to one end of the tilt base, and the base end portion of the support member is detachably fixed to the base base. Item 7. An X-ray incident angle setting mechanism of the minute angle incident X-ray device according to any one of items 2 to 6. 8. The minute according to claim 2, wherein the tip of the tilt angle setting screw is provided so as to be horizontally movable on the base according to the rotation of the tilt base. An X-ray incident angle setting mechanism of the angular incidence X-ray device.